Document mqD27v0mMy7o18K9Yg1BpeDnJ

{J p< / r ^ f - MONSANTO COMPANY / DAYTON LABORATORY / DAYTON, OHIO 45407 _______________E 5 C / D A Y T O W ______________________ (Department/Section) _______________ A N A L Y T I C A L ------------------------- (Type of Report) REPORT NO. : MDA-56.6 ^JOB/PROJECT N O .: 484.4390 DATE: 8 January 1985 0V0* PERIOD COVERED: ^ TITLE: Analyses of Wipes for 2,3,7,8-TCDD CN S O fc w w cu H w h sO o JC w Z* a w >> < u w a ua 0H 1< p AUTHORS: G. L. Thomas ABSTRACT: wipe samples from the Nitro plant were analyzed for possible concentrations of 2,3,7,8-TCDD. The results of these analyses are shown in this report. TECHNICAL APPROVAL: P. L. Sherman Sr. Research Group Leader APPROVED BY: O' R. F. Ivory Environmental Sciences Center Service Project Manager oo zz 2H > GC 0< O U S APPROVAL DATE: /~j' RESTRICTED DISTRIBUTION: (see over) COMPANY CONFIDENTIAL This document la the property of Moni an to Company and the recipient ia reaponaiblt for ita safekeeping and disposition! It contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthorised peraone or sent outside Monsanto Company without proper authorization. T x isso Monsanto //lYT0 MONSANTO COMPANY / DAYTON LABORATORY / DAYTON, OHIO 45407 ESC/DAYTON____________ (epartment/Section) a n a lytic a l (Type of Report) REPORT NO.: MDA-570 JOB/PROJECT NO.: 484.4340 DATE: 18 Ja n u a ry 1985 PERIOD COVERED: TITLE: ANALYSIS OF WIPES FOR 2 ,3 ,7 ,8-T C D D . AUTHORS: R. W. Noble ABSTRACT: Wipe samples from the N itro P la n t were a n a ly ze d f o r p o s s ib le co ncentrations o f 2,3,7,8-TCD D . The re s u lts o f these analyses a re shown in t h i s r e p o r t . TECHNICAL APPROVAL: P . L . Sherman S r . Research Group Leader APPROVED BY R. F. Ivory cJ Environmental Sciences Center Service Project Manager APPROVAL DATE: y-f7 - RESTRICTED DISTRIBUTION: (see over) COMPANY CONFIDENTIAL This document is the property of Monsanto Coapany and the recipient is. responsible for its safekeeping and disposition! Zt contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthorized persons or sent outside Monsanto Company without proper authorization. CONFIDENTIAL 4 I -i SU BJECT TO PROTECTIVE ORDER. c- DISTRIBUTION COPY NUMBEH 1-3 M. Townsend, Nitro Plant 4 F. E. Kearny, St. Louis-E3NA 5-7 T. Bistline, St. Louis-E2ND 8 G. Thomas 9 R. Ivory 10 Technical Reports Library - R2C 11 Central Files ABSTRACT ONLY h . A. Woltermann NOTE: Distribution of this report is restricted. Requests for additional copies should be made through the principal contact at the Monsanto location involved or the Manager, Environmental Sciences Center, Dayton Laboratory, Dayton, Ohio. ACKNOWLEDGEMENT Contributions of the following Dayton Laboratory personnel to this project are gratefully acknowledged: Analyses: Thomas H -IO M (C ) CQMBANiV^ CONFIDENT!At CONFIDENTIAL r n n m TO PROTECTIVE ORDER. ... ?11131 DOCUMENT CONTENTS Paga Cover Sheet . . . . . . . . . . . . . . . . ...................... 1 Document Contents ............................................... 3 Report ......................................................... Document Inventory Form ......................................... 4 9 Sample Receipt F o r m ................................................10 Chain of Custody F o r m ..............................................11 Analysis Request Form ..................... . . . . . . . . . . . 14 Monsanto Notebook Pages Fori a. Extractlon/PreparatIon ............................... 15 b. Analysls/Data Reduction ............................. 16 Instrument Logbook Pages ....................................... 17 Computer Output and Chromatograms ........................ . . . 18 Additional Documentation ....................................... 79 SUBJECT TO PROTECTIVE ORDER, m - - ' C11132 ANALYSIS REPORT FOR 2,3,7,8-TCDD IN NITRO SAMPLES INTRODUCTION On 27 Nov 84 eleven wipe samples were received for the analysis of 2,3,7,8-tetrachlorodibenzo-p-dioxln (2,3,7,8-TCDD). For internal purposes, the samples were assigned MRC Log #1-84-11-27-01. The samples were analyzed according to the September 1983 EPA Region VII method "Determination of 2,3,7,8-TCDD In Soil and Sediment". For quality control purposes MRC Method #Q7-QAQC-R3 was followed. Briefly this method requires that for every set of samples of the same matrix type a replicate sample, a low (9.6 ng in this case) spiked sample, a high (96 ng in this case) spiked sample, and a method blank must be analyzed. PREPARATION AND ANALYSIS (WIPES) The wipes were spiked with 24.0 ng of carbon-13 labeled 2,3,7,8-TCDD and 9.6 ng of chlorine-37 labeled 2,3,7,8-TCDD. Then ten grams of washed anhydrous sodium sulfate was added and the samples were stirred, allowed to stand and stirred again. Samples were mixed again immediately prior to addition of extraction solvents. The extraction process involved the addition of 15 mL of methanol (all solvents are Burdick and Jackson "distilled in glass" grads), stirring and the subsequent addition of 150 mL of hexane. The samples were then shaken for one hour on a'wrist action shaker and the extraction solvent removed. The solvent was then successively extracted with 50 mL of water, concentrated sulfuric acid (until clear), water, 20% potassium hydroxide and water. The hexane was then dried with 10 grams of anhydrous sodium sulfate. Each sample was then placed on the head of a mixed phase column consisting of (top to bottom) 2 g of silica, 4 g of silica plus 40% sulfuric acid, 1 g of silica, 2 g of silica plus 36% potassium hydroxide and 1 g of silica. The column was. eluted directly onto a column containing 2.5 g of Voelm basic alumina. The alumina column was first eluted with 10 mL of 2% methylene chloride/ hexane (v/v) and this fraction discarded. An additional elution was made with 15 mL of a 50% methylene chloride/hexarie (v/v) solution to elute the TCDD off the column. All samples had, 50 uL of dodecane keeper added to them and then were concentrated under a gentle stream of nitrogen and submitted for GC/M5 analysis. The GC/MS analyses were conducted on a Hewlett/ Packard 5987 GC/MS instrument. The analysis was conducted using a 60 m SP2330 capillary column. The mass spectrometer was operated in the selected ion monitoring mode analyzing for ions characteristic of both the native (unlabeled) 2,3,7,8-TCDD (m/z 257,320,322), chlorine-37 labeled 2,3,7,8-TCDD (m/z 328), and carbon-13 labeled 2,3,7,8-TCDD (m/z 332,334). 011133 cimtrnr m o n n T c r m n r n o n m STANDARDS Standard solution war prepared from standard that had bean cross validatad with a standard provided as a check sampla by tha PA. Concentration of tha internal standard conformed to tha level specified by tha method. RESULTS The results of tha analyses are given in tables 1-3. Tha tables also give all pertinent QA/QC information. oonns T T O T A EXPORT hksarto ro re w . rm LMrwnwr (icrura s5>mo BF NATIVE) .91* PF SLRnrCATFl 1.283 sam e anm l a2 3 a 5 & a7 aa #9 a to a it IW IK E WICH S P It t B SLRR EIT R m A N A lYTIttL 320 333- l m m CLFAA TO T D .l. DATE T I * 322 334 ACC 320 322 237 1289 333 334 j SC j BC j SC M O 11/27 1431 .7 5 .81 9 7. .9 9 -- 11/77 1431 .8 3 .7 8 98, .8 7 -- 11/27 1711 .7 3 .8 3 102. 9748. 9958, 9924, 1T0L 11749. 13321. 5718. 304293. ?U O ?S. 373984. 6709, 333 4 U . 274021. 330177. 8 m 417910. 332124. 412431. j BC j BC .7 8 -- 11/27 1734 .8 4 .8 1 9 6 , .7 3 -- 1U 27 1734 .4 9 .8 2 9 8 . 10119, . 12107. 7331. 414253, 340867. U 7 1 2 L 7830. 11350. 5K S , 391320. 335085. *09731. j BC 1.84 -- 11/27 1834 .8 3 .8 1 9 5 . 21O IL 2 46 3 L 11296. 360041, 3 I* 3 2 L 390*42. jK .9 4 -- 11/27 1853 .8 5 M 97, I2 W S . 14812. 6796. *20296. 3429R7. U 9 * # . j BC 1 .0 3 -- 1U 77 1913 .81 .8 0 H . 11422. 140T2. 7 7 *1 . 363177. 113714. 3906*3. j BC .8 2 -- 11/27 1931 .8 7 .81 96. 11323. 1 3 0 U . 6678. *31972. 377533. *67428- j BC jK j BC .7 3 -- 11/27 1953 .77 .8 0 96. .7 8 -- 11/27 7oa ,7A .7 9 94. 3 .8 7 -- 11/27 2053 .79 .8 1 112. 9381. 8503. 5 695t. 171 IS . 11472. 71784. 7398. *17618. 367745. 453625. 4819. 349120. 317922. 40*090. 31878, 373563. 2*2007. 33996. j rc 7 0 ,8 2 -- 11/27 2113 .81 ,8 4 1 0?, 6S302L 007964. 3001*0. 317881. 26S113. 317245. j BC . u 11/27 2133 .4 8 .8 0 101. 3780. 3394. 0 . 321927. 265654. 331*30, U fS a iTFD FOR a jT O IB J T l* w R A T I TO T (SUBTRACT .009 OF R/E 3225 M7TE COOES) I) ISTHTF RATIO CUT OF ACCEPTASLE KAMI VI I ACCIRACT OUT (T ACCEPTAg KARGE H*fTTO RJSUi P-MKT1. CAR SEPARATE IfICHIW AMO UORCI* D-^Pl ICAT<TMTEKLAfll F W E J BLAMt L.H-KATMTOT SFIKFS WCT DETECTED nWJfTECTI LIWT > HR FILERS*-TCm OOno CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER C111S5 1l * TABLE 2. CALIBRATION SUMMARY us/K* NATIVE TCDD 0.5010 5.010 50.10 1.2515 12.515 125.15 RRF (NATIVE) 1.0199 0.0902 0.8713 0.9030 0.9096 0.8882 DATE 11/27 11/27 11/27 11/27 11/27 11/27 TIME 1551 1611 1814 2013 2153 2213 RRF (SURROGATE) 1.318 1.224 1.238 1.240 1.329 1.350 GTT2X _^ U U I IIIV CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. .C11136 TABLE 3. QUALITY CONTROL SUMMARY ITEM SURROGATE ACCURACY SPIKE RECOVERY # DATA POINTS 14 2 MEAN S.D. 98.7 4.5 * * Not technically correct to report recoveries for internal standard calculated results. GTT3X j :CT7'/F C-'XH'tKi vs: oonns C11137 DOCUMENTATION INVENTORY FORM Monsanto Research Corporation Dayton Laboratory I. Sample Information Sample Identification: Number of Samples: II Analyte: 307 j K - T & P J> Matrix: f * s Method: J j 3j 7, F- 7~CP> in S a il a # * ! II. Documentation Control Copies Attached Initials (a) Sample Receipt Form // (b) Internal Sample Tracking Form --- (c) Sample Tags -- - (d) Airbill (Number P g #*> 4X77) '<' K *'l= xP ti& & I S su S * (e) Chain of Custody Form (f) Analysis Request (Log Number b 4 4 h X f ~h S S (g) Extractlon/Freparatlon notebook pages (NBP) $ 3 ) h / 3 S (h) Analysis nbp 2 7 3 a 7 7 S Instrument Logbook pages fS 'C ;7 0 0 \S Computer Data Files hard copy output Chromatograms s S 0s7U*V (1) Data Reduction NBP .:?<? 7 3 A 7 7 <j> Final Report 0 0 Additional Documentation S W S ' S juuT S' (note immediately upon acquisition) C r*3-r>a.t~t t/F 1 * 7 3 :iV j A I 7 3 2 S - //. / ^ Fila Complete O (signa tdre) CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER- , o r,0 0 9 - / - r C (dace) C1H38 yfei mu Sample R e c e ip t Form Monsanto Research Corporation Dayton Labo ratory Customer I d e n t if ic a t io n : N ( T o ________________ MRC Log Number: 1 ' ` W il - %-~l O I____________ A i r b i l l Number: ____________P C & H & 7 ~ 7 Date: f T T f o V 8 V __________________________ Sample R e ceip t In fo rm a tio n : (a ) Shipping Containers (b) Custody Seals ( c ) Chain o f Custody Forms Cd) Sample Tags (e ) Sample C o n tain ers ( f ) Agreement o f Sample Documentation ^ T n t a c ? ) damaged (d e s c rib e below) No. \ present <^aFsen^` (describe se a lin g below) in t a c t ____ ^ ^ p re se n j? p ferfnp absent absent N o .JL No. I I damaged (d e s c rib e below) No. ( ( no (d e s c rib e d is c r e p a n c ie s ) In itia ls A d d itio n a l D e s c rip tio n ( i f sample numbers not l i s t e d on c h a in o f cu stod y fo rm , l i s t here and c o n ta c t SMO) ) vrrH 1 o / io io -s 011139 UNIFORM STRAIGHT BILL O F LAOINO ORIGINAL NOT NEGOTIABLE p a y m e niTt i(Cc h EC a Od nNE) :Q::^ L ErTnT wE RTcncirS ottoAJR PE0004877 W S R A 'fltX P fils S C C & L IN T NUMBER ! FROM COMPANY N AU E (CONSIGNOR) k' n V mu, BOX OR TUBE Q a n O U N O TO COUPANT N AU E (RECIPIEN T) ':i * ~r -*7 b O RKL AIRPORT o a st, a ir p o r t 1! STREET ADORI SR STREET AOORLSB 1'7 I'* i ,J P.O. OR R E F E R E N C E N a " - .y .\j y o STATE IIP CODE (REOUlREOl Kr CITY r-- THJR PARTY NAME A K O 4D 0R C SS V --y * , STATE l*O*0RTA(.COCAiNOUia SH IPPER'S SIGNATURE COURIER GUARD SIGNATURA ROUT! DATI Tsr XX N0R-NK0T1A8L s a i V LAOm G S U U K T TO DESCRIPTION OF CONTENTS UNHOOKS OF CONTRACT SET FORT ON RE VERSE side of shipper s c o n . / " ^' a / /. r i f a // c_ n il mutuair, a>m mu 9000 < u m u K U T M * l e t i'ia f e a t orali M cw M noua lu if*A*poflatian U uma u gtaaiu tatua <1 oaeiuao ma tatua o1 i*a u o can i aaauiM* rataraa M l al ma i n a u r i eoa. ma uiippu nuaer araaa u h oacia rataaaao la a Usta aa aaatilaA u -- ---- F R EIG H T PIECES WEIGHT DECLARED VALUE 1 DIMENSIONS L WM _________ 1 _ J _____ I ` ADV. VALUATION in c iiL C w a "55" AAAOUN TTOTAL 4| |CHAMISy| MhNAiaSDiIirvDiOMcOIu*AOuITtC|HOolGrfNlcIoATHIn)AMilIoCOilTra*oAMa'iOumua*OiM*IumIcattI)oOAmv*ui W HITE. B U I MG MOUNTAIN STATE ENGINEERING SUPPLY SU BJECT TO PROTECTIVE ORDER. CHAIN OF U ftiO D t RECUD Mnc JOB HUHCEfl.......................................................................................................... CUSTOMER I'frPKCSCMTAri VL / f e y / S./W //Zes- ' CONTRACT NUMBER________________________________________________________MIC CONTRACT MANAGER __________________________________________ PLANT NAHE OR CODE / # Q - / / / 7~/fO HRC TEAM LEADER _________________________________' ` ( S p e c i f i c In fo rm a tio n on samples 1s a v a ila b le on a tta ch e d "Sample Id e n t if ic a t io n Lo g ") S ig n a tu re s Team Le a d e r V e r i f i c a t io n o f C o lle c te d Samples: Relinquished by: f fn if/ e t- Received b y: Relinquished by: Received b y : < ^ r ^ lo gged-ln-by: Received fo r A n a ly sis b y: ^ Method o f Shipm ent: Date Time /A u M A ' 7 ;a ? Number o f C o n ta in e rs : Remarks S p e c ia l In s tru c tio n s (Sample p re s e rv a tio n , s e c u r it y , d e liv e ry to , e t c . ) 00012 / S / S / U </ , r U/ ? J > __________________ A > y W , n / J / o _______________________ J 9 S /7 C1114 SAMPLE IDENTIFICATION LOG HRC Job H i . _____________________________ _ _ Customer R epresentative JC-. Contract No. _______ ,_______ HRC Contract Manager Plan t hetme or Code /^ o /r/fA i - o Team Leader ___________ ______ _ ________________ Samni 1r.g L o c a tio n j Rtf: Oate Type o f Sa.Ttple i 'tfunber Sanpled No. o f C o n ta in e rs 8 lk tJ g `79 /)/py M * */6 /do&-n* AJGfT*/ / `S'LCSS? 9h SotJTN SJsj-<.r1& y ssJ o* ? t js S Cn/?*tft? % A / o / e --t f */ *z \? < / *s ,/ / t s ia i. 1,/zC, ft/zfr / ft ft 11 n V ti n M J~rA <J* i ^ *4-4 * 7 /tSo/STV *3 W 7* *//?{**)<*}< 1 ' S' V yrfff V/S- S *, /O OfA/r&? '/ / h 11 n '/ n ff . it . ft ; '7 \ Analysis Reouf.red Sample re c o v e re d By ( I n i t i a l s ) and Cormenti Z. 3 ~7* T C O P u t. /% 1 } . n n t> * , ' - CONFIDENTIAL onn-13 C11142 DATI LOG NO. ANALYSIS REQUEST 7 ~!AJoi/f'W MONSANTO RESEARCH CORPORATION REQUESTER** DAYTON LABORATORY A ^ i+ s-. SAMPLE DESCRIPTION NUMBER OF BOTTLES: / j U \r CHARGE NO* ^UMBER OF SAMPLES / j // Z y / A J REPORT RESULTS TO* f il e s _^ C XTu ^ ANALYSIS REQUEST 1 / O f tsJ. >i 4 /v^ . tu *// / r ^ S X *OV*( fe 'Is Ja O ^ A J ^ Z }*~ Ir ^ J l j ( g 6 . " T 7 6/,. ^ f t < t r r K r K l* . U )q // 3 / r ^ SAMPLES FOR: O S m tiU ja l H {~ te REQUIRED ANALYSIS' RECORDED BY: & * `V aM < O SAMPLE LOCATION T" KNOWN HEALTH HAZARD PRESENTED BY SAMPLE: ^ =o t < ! > L 'llk s c f > .X REFERENCE TO PREVIOUS WORK (REQUEST#, JOURNAL,ETC.) COMPLETION DATE TIME ALLOTED FOR ANALYSES ANALYST . HOURS INST. TIME ANALYTICAL TECHNIQUE ' GAS CHROMATOGRAPHY ULTRAVIOLET VISIBLE INFRARED G EMISSION EDAXXRF * MICROSCOPY OTHER ---------- QUAI__________ SEMIQUANT. NMR HPLC XRD ICP ATOMIC ABSORPTION MASS SPEC -^GC/MS AUTO ANALYZER ______ QUANT_________ REQUIRED QA/QC _______& \?< > -SAM PLE DISPOSAL: AFTER REPORT COMPLETE DISCARD D RETURN HOLD FOR O 30 DAYS THIS INFORMATION MUST BE SUPPLIED BY ANALYSIS REQUEST ORIGINATOR 0 6 0 DAYS c i n tre on MONSANTO COMPANY SUBJECT /JiTfO l p t i ' JO B NO. ikOM X Vb 4 4 3 ? / 9 ^i'ox'i'A, /^ W l/S *. P R E P A R E D BV (SIGNATURE) ~ U udr S d a N? 2831613 date ^ 7 A lv o Xl>\Lc Afe f J q u 05 Wo. -----&>k Ma------ Attiro L d t 'f e s ~Dtu :Zl> c Wo. UT 379 U T 3(80 trr 3ifl /TT 3 I 8 2 o r 3/0 3 D T 3/</ uT 3 l8 r UT 3l8fc U T 3 18 7 u rsiS S U T 3/ 8 9 n r 3\ 9 0 UT ZI 9 I UT 3i92 fitfa TP r ------------ 1 . ii- H I P h 'JC itX Dnf i/o h t keift,s 779 ) di 3 N E [V< 7 <A-A/_ a y A/orfh n il / BS6. </ e r . PII* r M A / * / c arner M 'A / l fle tti /Poe*. ot/T u / * lt ti- V d a C e / b , F t'rt (L fy ll M A / t t f C i d Fy'rc M< l i OC. S S / 0 Cuffie r f ? r , W , f i fo d L l& tj M S . u n ' f i f e U H 3 rd (<sd M s L o SpiKe hh~ S ftfc t 6 n h j e t S lo e (our 0 ______ fcto/%1 f'- t d Wrtiuc. C* tur. (O y ,Com/o0 3 y _gftcAs<* fk recent y j lOt/ o f M kr*4 Sfa yy 'y ? , - J L y f faa-cxL^** y/ / /O u! Uu v/ y // i/ /- ~ _ y y f* safadu->>fh . / U 1 .iV d ttA t. 7ZOO / / /> /'so-oc'&ter c o c c e . z & k c c k p u d p r e p a i d , / h 'S i c / H 4 .* / te f~ & ch & & A - H ./ S C rib e d t o n p a g e . % 8 3 ? l "0 Tflty U J C C C L O o C C - d l u p in " i c ( b qnd C L 3 Z m os - t t c z r t f s T a td z rd s - SU B JE C T TO PROTECTIVE 0 r >ER. 0 0 0 15 ABAS ANS UNDERSTOOD S T C11144 O A TE P X 1 5 3 *0 Monsanto ^ /1 ___________ _ _ _ ) l O 4 MONSANTO COMPANY / DAYTON LABORATORY / DAYTON, OHIO 45407 ESC/DAYTON____________ (pepartment/Section) ANALYTICAL (Type of Report) aa i CO * n A C\J Q o Li- tO LU a_ <U Lu -- O ZJOO to *-> to >- 2 --1 <z O C 'V) w i 4S i or*. LO 1 <a > OO 2Z HX 2 A O u REPORT NO.: MDA-570 JOB/FROJECT NO.: 484.4340 DATE: 18 Ja n u ary 1985 PERIOD COVERED: TITLE: ANALYSIS OF WIPES FOR 2 ,3 ,7 ,8 -T C D D . AUTHORS: R . W. Noble ABSTRACT: Wipe samples from the N itro P la n t were a n a ly ze d f o r p o s s ib le concentrations o f 2,3,7 *8-1 0 0 0 . The re s u lts o f these analyses a re shown in t h is r e p o rt . TECHNICAL APPROVAL: P. L . Sherman S r . Research Group Leader APPROVED BY: ___________________ R . F . Ivory c) Environmental Sciences Center Service Project Manager APPROVAL DATE: /-> 7- _____________ RESTRICTED DISTRIBUTION: (see over) COMPANY CONFIDENTIAL This document is the property of Monsanto Company and the recipient is responsible for its safekeeping and disposition! It contains CONFIDENTIAL INFORMATION which sust not be reproduced* revealed to unauthorized peraone or sent outside Monsanto C o ^ a n y without proper authorization, CONFIDENTIAL C10904 SU BJECT TO PROTECTIVE ORDER. DOCUMENT CONTENTS C o v e r S h e e t .................................................................. Document Contents .............. Report ....................... Document Inventory Form ........ Sample Receipt Form ............ Chain of Custody Form .......... Analysis Request Form .......... Monsanto Notebook Pages For: a. Extraction/Preparation b. Analysis/Data Reduction Instrument Logbook Pages . . . . Computer Output and Chromatograms Additional Documentation . . . . Page 1 3 4 11 12 13 16 17 20 23 29 154 S B C10906 ANALYSIS REPORT FOR 2,3,7,8-TCDD IN NITRO SAMPLES INTRODUCTION On 1 Nov 84 thirty-five wipe samples were received for the analysis of 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD). For- internal purposes, the samples were assigned MRC Log #1-84-11-01-02. The samples were analyzed according to the September 1983 EPA Region VII method "Determination of 2,3,7,8-TCDD in Soil and Sediment". For quality control purposes MRC Method #07-QAQC-R3 was followed. Briefly this method requires that for every set of samples of the same matrix type a replicate sample, a low (9.6 ng in this case) spiked sample, a high (96 ng in this case) spiked sample, and a method blank must be analysed. PREPARATION AND ANALYSIS (WIPES) The wipes were spiked with 24.0 ng of carbon-13 labeled 2,3,7,8-TCDD and 9.6 ng of chlorine-37 labeled 2,3,7,8-TCDD. Then ten grams of washed anhydrous sodium sulfate was added and the samples were stirred, allowed to stand and stirred again. Samples were mixed again immediately prior to addition of extraction solvents. The extraction process involved the addition of 15 mL of methanol (all solvents are Burdick and Jackson "distilled in glass" grade), stirring and the subsequent addition of 150 mL of hexane. The samples were then shaken for one hour on a wrist action shaker and the extraction solvent removed. The solvent was then successively extracted with 50 mL of water, concentrated sulfuric acid (until clear), water, 20% potassium hydroxide and water. The hexane was then dried with 10 grams of anhydrous sodium sulfate. Each sample was then placed on the head of a mixed phase column consisting of (top to bottom) 2 g of silica, 4 g of silica plus 40% sulfuric acid, 1 g of silica, 2 g of silica plus 36% potassium hydroxide and 1 g of silica. The column was eluted directly onto a column containing 2.5 g of Uoelm basic alumina. The alumina column was first eluted with 10 mL of 2% methylene chloride/ hexane (v/v) and this fraction discarded. An additional elution was made with 15 mL of a 50% methylene chloride/hexane (v/v) solution to elute the TCDD off the column. All samples had 50 uL of dodecane keeper added to them and then were concentrated under a gentle stream of nitrogen and submitted for GC/MS analysis. The GC/MS analyses were conducted on a Hewlett/ Packard 5987 GC/MS instrument. The analysis was conducted using a 60 m SP2330 capillary column. The mass spectrometer was operated in the selected ion monitoring mode analyzing for ions characteristic of both the native (unlabeled) 2,3,7,8-TCDD (m/z 257,320,322), chlorine-37 labeled 2,3,7,8-TCDD 2,3,7,8-TCDD (m/z 332,334). T0 pr o t e c t iv e o r d e r . C10 907 STANDARDS Stan d ard s o lu t io n s w ere p re p are d from sta n d a rd s th a t had been c ro s s v a lid a t e d w it h a s ta n d a rd p ro v id e d as a ch e ck sam ple by th e EPA. C o n c e n tra tio n o f the in t e r n a l sta n d a rd conform ed to the le v e ls s p e c ifie d by th e m ethod. RESULTS The results of the analyses are given in tables 1-3. The tables also give all pertinent QA/QC information. _,,^'JDiNTlAL SU B JEC T TO PROTECTIVE ORDER. noon: AA nAnn to o data c e r a r m&MTO OPSW. DAYTONIMCRATCRY T Aa\- 1 x c a w : SP2330 OF NATIVE: ,973 RF SLPBKATEl 1.324 SAffLE MIWFS WAffi S fa ETTR XT PP9 ANALYTICAL 320 332 I mm CLEAN UGHT TdB ILL. BATE TIX 322 334 ACC 320 322 257 3284 332 331 M LAWFUL IA j LAWFUL IB J LAWFUL IB L j LAWFUL 1C J LAWFUL 1CP J LAWFUL 2 j IAWFTI |. 2 H j LAWFUL 3A J LAWFUL 3A S J LAWFUL 38 J LAWFILL X J LAW FUL X L J LAWFUL A4 J IAWFIU *R J LAWFUL AS H J LAWFUL AC .1 LAWFUL ! J LAWFUL 58 J 1AWFUL M i 91At* j SC 10.A10 X 10.210 X 11.270 X . 10.020 X 10.430 X 10.250 X 10.410 X 9.940 X 10.150 X 10,310 X 10.770 X 10.5*0 X 10.>00 X 10.290 X 11.020 X 11.5*0 X 10.110 X 10.410 X 10.050 X 10.000 W. 7.31 9.87 t,42 2.23 .28 9.19 .14 .14 .2 3 .83 1.20 m m 9.41 .14 TO Vt NO m .14 11/05 -- 11/05 -- 11/05 -- 11/05 -- ll/CS -- 11/05 -- 11/05 -- 11/05 -- 11/05 -- ll/C S -- IV05 -- 11/05 .13 )t/05 .17 11/05 -- 11/05 -- 11/05 .08 11/05 .09 11/05 .09 l!/ iS .04 11/05 0100 .88 0120 .92 0140 .83 0200 .81 0220 .80 0305 .74 0325 .81 0345 .73 0406 .84 0425 .81 0510 .74 0529. . .79 0549 1.24 0409 l.tB 0429 .S3 0714 .74 0734 1.10 0754 .90 0815 .72 0835 1.14 .81 99. .79 100. .90 94. .81 97. .82 98. .81 99. .84 101. .91 101. .8? 99. .82 101. .83 107. .83 102. .83 102. .82 94. .83 104. .84 112. .85 112. .84 1(15. .84 110. .83 103. 9308. 10543. 4421. 183778. 1W80. 197444. 1 271499. 331487. 157882. U0549. 91898, 115793. 598907. 721294. 318020. 155155. 134034. 149042. 97974. 120374. 55704. 17X32. 151214. 190423. 114939. 143415. 44204. 145743, 124212. 153195, 15714. 20590. 12100. 149523. 143702. 177594, 414889. 512423. 21X77. 133019. 113*09. 135802. 7138. 9792. 5905. 1*9050. 124292. 153933. 7014. 8151. *040. 1*3384. 123134. 151914- 11143. 13833. 10304. 1*5443. 122432. 1*8933. 77784. 34350. 17421, 104397. 83700. 100340. 59021. 743*3. 34154. 144212. 122225. 147721, 8894. 704*. 8719. 144274. 137753. JWM9. X 9448. 7995. 0. 132433. 117207. 142754, I 513720. 418539. 290935. 154220. 127707. 1529*5, 8990. 11X1. 7781. 149937. 130522. 153119. 7947, 7715. 0. 284380. 221554, 240291. I 8272. 9185. 0. 758033. 212445. 251975. 1 5359. 7AA1. 0. 212549. 144153. 198014. 4901. *314, 0. 233438. 193055. 232914, J CCRAECTED FOP CONTRIBUTION BY N A TI TOOT I9JB TW T .009 OF p/E 322) HUE COESi . I : ISOTOPE PATIO CUT OF ACCEPTABLE RAWS y i : A cafiA cr our c f a c tep ta r e w e H&tfETWJOFLA# PaPCRTTAL SCAN RIPARATEXTWIW ANDWSOF P=HPlirATEtlTPiS.t) FS=FIFLO FLAMC l .# n a ti T a n s p ik e s (C riflT IFTHCTEB O L rF T E a i U N IT xw F IL E O E -TCD002 C O N F ID E N T IA L s u b je c t t o p r o t e c t iv e o r d e r . nnr*r>. C10909 TOT PAIAREPORT WfSAKTO CBM NY. DAYTSI LABORATORY T 1 LOi j T) OCCOUKi: SPTJ3C Rf NATIVE: .755 9AKSATE: 1.023 awiF. irnp? ---- . ETTR KTH) W ILL 69 J .W ILL 6 H J .W ILL 7& J JW IL l 7B J W ILL 7B L J .W ill 70 J NITROSITE 1A .J N1TR SITE 1AA J NITROSITE 18 J NTTROSITE IEH J NITROSITE IC J NITROSITE ? U NITROSITE 21 J NITRO SITE 3fi J NITRO SITE 3B 1 V NITRO SITE A J NITRO SITE J NITRO S ITE J mitro s it e ra 0 MITRO SITE 5C J MITRO SITE 6 J MITRO SITE 7 MITRO SITE 9 J 9/ r* J GRATS irr CLEAN KMT BC 10.690 SC 10.710 PC 10,740 sc IO..TM PC 10.590 EC IO.CT BT 10.610 BC 10,3M PC 11.410 BC 9,950 PC 11.040 BC 10.400 BC i i . n o BC U.O M BC 10.320 PC 11.660 PC 10,990 PC 11.560 BC 1 1 .5 BC 10.290 BC 1 0 .4 PC 10.300 PC 11.060 BC 10.000 m TOT D.L. .11 -- 8.19 -- .11 -- NS -to .94 -- 1.76 -- -14 -- ND .12 W) .48 9.29 -- HI ..34 HD .46 1.52 -- NS .13 .14 -- MD .09 NO .0 * .91 -- .74 -- .47 -- 10.34 -- HI .67 ND 20.9 NS .03 - SW analytical 350 332 t CATE T I* 372 334 ACC 11/05 HUB 11/05 11/05 11/05 11/05 l\"/05 11/05 11/05 11/05 11/05 11/05 11/05 11/05 11/05 11/05 11/05 11/05 11/06 11/05 11/05 11/05 11/05 11/0? 1902 -81 1927 .73 IBM .84 1909 .84 1928 .73 2009 .70 2029 .84 2049 .87 2109 .85 21 .75 2210 ,82 2230 .81 2251 . -78 2311 .71 2331 .76 0158 .83 02)8 0.00 0239 .72 0259 .77 0319 .81 0405 .75 0425 .67 0445 0.00 CMS H 4 .79 94. .90 90. .78 93. .77 94. .77 97. .77 102. .78 98. .81 98. .76 107. .81 99, .77 96. .82 107. .84 115. .78 122. .79 104. .80 n o . .80 n o . ,78 10?. .73 103. .79 106. .79 m . .74 97, .81 147. .78 n o . 320 322 2279. 233. 182902. 252199. 2779. 3319. 2258. 2693, 19379. 26564. 29827. 42418. 3061. 3627. 2673. 3072. 2516. 2960. '63*80. 84734. 2819. . 3438. . 2581- 3190. 4469, 5694. 3 1 . *755. 3550. 4663. 2164. 2599. 0 , 2195. 19078. 26403. 19325. 25090, 10611. 13035. 2*0320. 320370. 5078. 7535. 0 . 36039. 0. 0, 257 -- 338+ 332 --. -- 334 K --_ 2701. 55395, 63*33. 80794. 86382. 53406, 70261. 87733. 2556. 63706. 73302. 93511. ft. 53432. 65369. 85687. 9399. 58260. 67CT. R7495. 14043. 503*9. 52535, 68411. 3137, 59;. 65114. 83298, 0. 57639, 63950, 79259. 0. 1*045. 13370. 18171. 28852. 20723. 2OT6- 28326. 0. 20721. 22Pf, 79628. 0. 16760. 17274. 21R13. 3370. P980. 8725. 10429. 0 . 79913. 70151. 90*22. 2*76, 75712. 78372. 99650. 0 . 66856. 65753. 82695. 0 . 8 5 9 . 65753. 87695. X 8619. 57525. 0573. 77400, 8327, 69985. 72387. 93277. 5434, 67502. 68351. 87047. 92691. 75223, 73061. 92*81. 0 . 73110. 24/31. 33494. 3956. 2997. 2230. 2745. XY 0 , 7 1 8 . 69795. 89619. I CORRECTED FOR CONTRIBUTI BY NATIVE TO T (SUBTRACT .00? CF /E 322) NT;TE CODES: I ! ISOTOPE T IC CUT CF ACCEPTABLE RANCE Y : I ACC.SACY OUT OF ACCEPTABLE RANGE ^ T H ID BLAW p=?art: a l scan SEPARATE WEIGHING AND D*3.R.TWE[INTEW.AB1 FB*FIEU I BLAHC L .^ T IV E TO T SPIKES NWOT [ETECTED tW ETO TJCN LW IT >R P IL E ."? -TO1D03 M * t '< *y CONF SU BJECT TO PROTECTIVE ORDER, C10910 TOT) WTA (SPOTT flrssarro am s.ir, nenon laroratory i A8.i l GC C fi. l: SP2330 Rf KATI'^t ,7 ? l RP aSOTGATii .ftt SW FLF MWFR WAMS EHR WET KTMJ CLEAN UCHT PPB TOT) IL L . SIRS ANALYTICAL 020 332 X DATE ru e 222 334 arc 320 322 257 328+ 332 334 N SiTTRO J SC 10.430 .84 11/9 1431 .8 2 .75 103, 1772. 1445. 1331. ' 4741. 3115. 6340. XITRC 10 J BC 10.300 m .98 11/9 1432 H H .87 127. 0. 0. 0. 2334. 2334. 2498. I nitro aio l J 8C 10.200 l . n -- 11/9 1512 .7 4 .7 4 73. 2063. 2483. 1913. 2 W I. 4030, 5313. ' NITRO !! J DC 10.370 3.70 -- 11/9 1332 .71 .73 84. 4SI91. 675S4. 22778. 32714, W181. SK 7 7 . XITRO # :2 .J BO 9.830 .39 -- M/9 1333 ,87 .82 113. 8174. 9422. 4420. 29160. 31437. 33314. ICTRO I I ? H J BC 9.830 11.23 -- 11/9 1633 .74 .73 93. 2210. 29318. 11939. 3844, 7104. 9109. KJTBf! 113 J BC 10.MO .22 -- 11/9 1837 .4 3 .82 IC S. 2051. 3030. 2413. 29933. 33994. 41333. NITRO I I * R J BC 10.500 .23 -- 11/9 1737 .48 .8 ? 103. 1814. 2451. 2243. 25770. 27287. 33794. J J BC 10.000 W .07 11/9 1717 HH .79 103. 0. 0. 0. 29767. 32990. 41748. I * CXSECTFD FOP C W TR IB JTI BY SAHVF TOT) (S J T W a .009 OF K/E 322) te arats: I : ISPTCPE RATIO OUT CF ACCEPTABLE RANGE Y : X ACOPACY CL!T OF ACCEPTABLE Ra*CE fi^ETUfi B.eMC PARTIAL SCAN feSEPAAATE ICICHTNG AND KR K IP P=Ti PLICA7F ( INTERl-AB) FfcftELD EJWi L.W dttTIUE TOT) SPIKES KD=ST FFTFCTED urndl=o etec tiw KIAR FUEMWi TCT0A CONr SU B JEC T TO PROTECTIVE ORDER, n( C10911 TABLE 2. CALIBRATION SUMMARY ug/Kg NATIVE TCDD .501 5.01 50.01 1.25 12.5 125.0 .501 5.01 50.01 1.25 12.5 125.0 RRF (NATIVE) .836 .662 .703 .729 .721 .677 1.11 .909 .944 1.04 .923 .923 DATE 11/9 11/9 11/9 11/9 11/9 11/9 11/5 11/5 11/5 11/5 11/5 11/5 TIME .13.51 14.11 16.14 17.58 18.19 18.39 00.38 02.43 04.47 06.52 08.55 09.15 RRF (SURROGATE) .925 .884 .940 .951 .952 .901 1.27 1.29 1.40 1.37 1.29 1.32 CONFIDENTIAL SU BJECT TO PROTECTIVE ORDER, cl091a TABLE 3. QUALITY CONTROL SUMMARY ITEM" SURROGATE ACCURACY SPIKE RECOVERY # DATA POINTS 35 10 MEAN + S.D. 105 10.8 * * Not technically correct to report recoveries for internal standard calculated results. GTT3:GT n On-j Q SUBJECT. TO PROTECTIVE O R D ER C10913 DOCUMENTATION INVENTORY FORM Monsanto Research Corporation Dayton Laboratory I. .Sample Information Sample Identification: / I Number of Samples: 3 5 3 Analyte: J 2 , 3 . 1 , ^ 7 - h J ) Matrix: Method: - D t t * i o a t ; c/O o f - 2 , 3 , 1 . ? 7 >~ 6 o i l * S til ii n i o t II. Documentation Control Copies Attached Initials (a) Sample Receipt Form (b) Internal Sample Tracking Form (c) Sample Tags (d) Airbill (Number ) (e) Chain of Custody Form (f) Analysis Request (Log Number (g) Extraction/Preparation notebook pages ( N B *2) f?* P --^ (h) Analysis nbp 2 6 ? 7 > ? p - . 2 ~ '5ve7v*2 Instrument Logbook pages Computer Data Files hard copy output Chromatograms (i) Data Reduction NBP (j) Final Report ^ (k) Additional Documentation (note immediately upon acquisition) -- ifVjJ __ --. z e iA i/^ /O w IV Jt S ^UJ>J Jj =IAN F /e ^ rJ J S /0aW j <1 File Complete signature) n o m jL / C G W ir4 .'Id -l'li' ~ SU B JEC T TO PROTECTIVE ORDER, jtA-gr (date) C10914 Sample R e c e ip t Form Monsanto Research C o rp o ra tio n Dayton Labo ratory Customer Id e n t if ic a t io n : NJ t Q r i____________ MRC Log Number: 1 - 9 4 - i ! - .O I - L A i r b i l l Number: ________ ^ ________________________________ D a te : ___________ f r J n \ i . P 4 ________________________ Sample R e c e ip t In fo rm a tio n : (a ) Shipping Containers (b ) Custody Se als ( c ) Chain o f Custody Forms (d ) Sample Tags (e ) Sample C o n tain ers ( f ) Agreement o f Sample Documentation in ta ct present ('presen^ (^pfffSntN 'T n ta c-f) Q yes^ In itia ls damaged (d e s c rib e below) N o._5_ a b s n t^ (d e s c rib e ^ __ s e a l i n g below ) in tact absent NO.-3 absent No-?L damaged ( d e s c r ib e below ) N o jy & L no (d e s c rib e d isc re p a n c ie s ) A d d itio n a l D e s c rip tio n ( i f sample numbers not l i s t e d on c h a in o f custody fo rm , l i s t here and c o n ta c t SMO). nn n-f 2 CGPsu-*'!^`c.''UJNTIAL SU BJECT TO PROTECTIVE ORDER- C10915 MRC JOO Hl.'MOCR_____________________________________ CUSTOMER I'tPRCSCMTAilVE / V / t s * # CONTRACT NUMBER ___________________________________ MRC CONTRACT MANAGER ________________________________________ PLANT NAME OR CODE V/T/W MRC TEAM LEADER ( S p e c if ic In fo rm a tio n on samples 1s a v a ila b le on a tta ch ed " Sample I d e n t if ic a t io n Lo g ") XD- S ig n a tu re s Date Time Remarks Team Lead er V e r if ic a t io n o f C o lle c te d Samples: R e lin q u ish e d by Received by: fa /^ o /y) /O' v i ' p3 Relinquished by: Received by .................................................................... M .... Logned~1n-by: Vj r-- Received fo r A n a lysis by: ________ ____ . ri tTtT__Leii _n__^T -r----- Method o f Shipm ent: Number o f C o n t a in e r s : O ------------------------------------------ --------- - - -------- ------ -- L-- LU W S p e c ia l In s t r u c t io n s (Sample p r e s e r v a t io n , s e c u r i t y , d e liv e r y t o , e t c . ) _______________________________________ | ^ O MRC Jet. Hi. Contract No. Plant or Code N rrfo o SASf-'LE i Ot'hTl FI CAT IOH LOG Customer Representative Pla/2*: MRC Contract Manager Tea.n Leader __ SAMPLE iOEST]Fi CAT ION LG MRC Jc- Hi. -/ --------------- Contraci No. ____________ P la n t hc'me or Code (to C u s to d i" R e p re s e n ta tiv e fr W f c t T ^ j iuogN-JiMRC C o n tra c t Hanauer Team Leader Samrii/.g Loe* t'"or. 'k \3> se. 5 ft > (o cv is u 'O ; Ri"- i Ga te Type of Sartie fSur.t-er Sampled No. of Containers; 0.0 rJlTTW 501U 1 Analysis Required i i { .. ! ni !1 i .i !! 1 ii li M `I \y u _ L 1\ f r i1 ! ! ! i ! L ._L ` !i Sample recovered 6y (initials) and Coment! _ .. . \a ! ! i ! ; _ \"A ! 1 ss ! ! t i r* -7 !. \ ! ----1--'---- 5 fi 1 1 1 1 .1 i i 11 . . \j j i 1( . j .! ---- - !i ,___ _ ,, -- ) A T 1 C ^ f ^ v i^ ;4--s'-'*.."M-1-'* * J. IQ PRTECTTiSv i siiBJECT ^ -- - E -- 1_______ V~ ^ ^ j 077 -- -- J S ) o<t gLj C10918 DATE ANALYSIS REQUEST LOG NO. MONSANTO RESEARCH CORPORATION REQUESTER" DAYTON LABORATORY / ). h - ,, / + ! , * A 1_ f CHARGE NO." SAMPLE DESCRIPTION NUMBER OF BOTTLES; : < 1? H, / T As 7 !3 i i l"C " o 7"A " NUMBER OF SAMPLES IA 7 IB 7a HA 6. 3A bA } 3 --s-'i--^ c x i? 1; , /" to II Ua sc 1C CA a HC REQUIRED AN ALYSIS** ' j J 7 ^ ___ -- -5 ,'V-/' ( n,< report resul FIUS/KULIK rt X f, jXt, ' ANALYSIS REQL FILES/ / ) ? X . ^5k-r~ O --- 1 ' * Z . v / r v, cSAMPLES FOR / v ti SAMPLE LOCA' ?7> . KNOWN HEALTH HAZARD PRESENTED BY SAMPLE: /tS > __ L- t-' j *. * U/*-'f s' REFERENCE TO PREVIOUS WORK (REQUEST#, JOURNAL,ETC.) ** COMPLETION DATE TIME ALLOTED FOR ANALYSES ANALYST HOURS INST. TIME ANALYTICAL TECHNIQUE ** GAS CHROMATOGRAPHY ULTRAVIOLET VISIBLE INFRARED EMISSION EDAXXRF MICROSCOPY OTHER __________ QUAL_________ SEMI QUANT. NMR HPLC XRD ICP ATOMIC ABSORPT MASS SPEC ~vJ3'GC/MS AUTO ANALYZER ______ QUANT _____ REQUIRED QA/QC -- ^ ^s c' r ,r .,rw m>-- C O l- ik l 'j ill iI i SUBJECT TO PROTECTIVE-ORDER, SAMPLE DISPOSAL: AFTER REPORT COMPLETE D DISCARD sal11 Q RETURN HOLD FOR THIS INFORMATION MUST BE SUPPLIED BY ANALYSIS REQUEST ORIGINATOR 30 DAYS C109TS DAYS MONSANTO COMPANY SUBJECT /[fife)S (is - L.awt( S t jo b n o . P R E P A R E O Y (S IG N A T U R E) HM . 43% N? 2831624 OATE Z o Vou 8 ' s>\lc O^Wob Ajo I Afa./ g y Z o it . N o . v T 30*-} 1 _ L . na I . J. 4 3 . e .B HH 1 e vr 1c . - M I OL _ *0 . 0 /4 - 54 _ . ari 3 -p > - 52 3 53 < . 5V MB 5< <rr~ 57 5jR 5 *9 TT30-T3 4A M C. 5>f 5^ tfai t r y Jji'jro 5o)l6 ** L *ai1( " ** -- * f l " . to -- -------------- - / 0 L o S p JC t fe p lr c a 'fe M' f fy / iW e k O 5 * 'f e V' / ' V r # 7k. y by --T^ Cff^ (^J/rbCs V-- / h u r .l / l * t -V A irtii/o t u r . fiN & l lO 'H I 1 0 .7 1 Co ( 7 t7 JC / / d iK ia ^ V rz n e v r/ 1 1 .1 7 v/ kX P u ln i- r-a i il. O .O . .sM M c / f c f o - /3 / 7 ,2 5 ' 0 .H I J/O O u .1 / T ry *. J 1 / / </ ; id a s 1( 7 ,3 / fo *7 7 / O .S (0 5 C 7 yi J/ J ; . / ; If ? .3 9 //- 0 MCtyu ( / / ,4 7 w /y l(Ll I7-<T/T l/ { /) { i i V ii/ !5 it (fi `! i `i*i ^ - SUBJECT TO PROTECTIVE ORDER, G10920 `-1l 0 0 0 1 7 MONSANTO COMPANY MONSANTO COMPANY N? 2831626 SUBJECT JO B NO. - s 'a s MONSANTO COMPANY P R E P A R E D 0Y (S IG N A TU R E) N? 2637230 D A TE TOT SM XKFT SSKTOO W . 0*051ll*BMf 1 X C U flE SP2OT W 4T1WI .773 V SdSffiMEi 1.334 W K O m MW LUOFUI.It J iMcnu.ti J ina tii J w m fiil ic te . f i o . i lLuaeWrTnLil, 27h lUFIU.3 J J J J J LdCFIlL 3* J LMfflFia .1 lU F lU . X J wtsCFlll. X L J LwrilL 4 J IM TtU 4 J LWCFIU 4 H J I.KFTU. *C LtFM.54 Lxm a tu m i 4 J J J .J BU* J OtMS ter CUM to o X io.*io K 10.210 W2X li. r 10.0 X 10.430 C 10.250 X to.no x 10X M W . IW X 10.310 X 10.270 X 1C.SU K. 10.400 X 10.2 X 11.0 R 1I.SU X 10.110 K 10,410 R 10.050 X 10.000 SW K * seme*, 3 332 X TOT tu OME TI* 322 4 ttz 322 257 32* 332 .134 M .1 tue 0100 M 7.31 -- *.*t -- 11/05 01 II/CS 01U ..X0 . . TW , 10543. 4421.18B7W.1400M. 197444.1 . 100. 2714. 331167.IST.11054*. *18*8.1157*3. .X *4. 599907. 7217*4.3180. 155155.114034.149042. 1.42 -- UrtS 0200 .1 .61 f. 97774. 120374, 57M. ITO.15514.1. 2.23 -- IW 02 .60 .X n. 114*39. 1U4I3. 44204.1*7. 12X12.1531*5. . -- 0. 1* -- .14 -- li/es a j .74 .i . 15714. TO90. 17100.I4*S3.1*37. 1773*4. 11/05 iw 0325 QMS .61 .73 .94tot. 10.91 ). 414889. 312473.216577.1X01*.'.1340*.135*72. 7136. *772. S9. 11*950,124292.153*53. t.14 6 8-- IW .64 , ? . 7014. 6151. 46U. 1*5381.125134.151*14. .23 -- 11/ 01 .61 .X 10t.* UIM. 13R33. 10304. 14*.122432. *,18731. .83 -- 1. -- tu 10 .74 11/ 2* .7* .83107, . X 10t 27784. 3430. 17421,1647*7, 83706.lOdOW, 59021. 74313. 3*134.144212.177725.1*7721. W .13 IW .17 1 1 / 4* 1.24 XIX. out 1.19 .X 74. PP94. 7044. 8719.14**.177753.IMA, t *446. 7**5. 0.1X433.117207.142754. I M I -- IW 64 .83 .Kt 104. 3139. 4185.290*35.154270.127707.152*43. .14 -- IW 0714 .74 .84II2. B**0. DXI. 7761.14*937.1.W72.15511*. X .06 1t/ 0734 1.10 .35112. 7*47. 7715. 0.784380.XI54.2407*1.t X .0* IW 0754 : .84T. 87*2. IBS. 251*73.0. 25SC33, 2124*9. I X ,0* IW 13 ,72 .84HO. 33*. 7441. 0.212349.144151.1*6014. .04 IW 005 1.14 .83iOll 501. 4314. 0.mu. !**.2X914.1 3221* c o s s e r o F cd c* : w t i w w t o t o jw m c t .cot cf */e CTTOTES 1t ISOTOPS RATTO CUT CF flOTTMLE MCE vt X m u e r TUT er frrnafcE M CC iweth neue WMTIK. SOU ft**MEict:C WCF WXKITtIllTP.0 FKIM 1U* L .w T i\ < r o c gt*G o ct irro ro CWTCT1W Ltwrr JJ fiLEwtrana- \ /S" V ~ N V?. ,, ' - a mv >y oUBJECT IO PROTECTIVE ORDER - C l 0923 n e AO a n d U N D I6 IT O O O Y OA T E il SU B JEC T JO B NO. MONSANTO COMPANY r 5 ; P R E P A R E D BY (S IG N A T U R E) N? 2637231 d ate TOT WH W W iRAttTSDttwr. MTTfIWCMW T fc *,.* 1 L t ., n rt. cx-jtk 'vnx Vt TTWi .735 w sjttj :.ea ' EK 1 wre SI AffVF in n Em rer rei AtUnirJL r re a iut IOTI ICS n.u WIE TIW 332 t 334 KC 320 322 257 321* 332 334 a ffiti j .a ffla ut j .a ffla 74 j .iffIII 71 j teffIli 71L j a ffla 7(1 j (ITO SITI 14 j TRI SITE IM j CTWSITE II j V1T30SITF UH j <1783SITE 1C j TJtt 'ITT J ,i vino siti n. j VITO SITE 34 j TITRI SITE 38 NJTRl SITE 4 j TIISOSITE TITR1SITE VITTOSITE *i j j VITTOSITE SC j vino site 4 j VITTOSITE 7 j VITO) SITE 8 i* j X X C Kre 10.4 10.710 10,740 10.W 10,590 .11 0.19 -- ihm iw 1807 .*i .79 94. 1877 .73 . 90. .11 -- 11/ 1841 .84 .n n. K) .10 1/M 19 84 .77 91. .94 -- u/m 19 .73 .77 97. 2279. 28. m i. 55395. 4W3. 794. 187:. =7199. A43C. SW*. 70341. 87733, 2779. 3319. 2554. 43704, 7330?. TSU. 2S8, 243. 0. 58472. 45349. 85437. 19379. 24544. r*T. 58240. SORTI. 495- re r re io.reo 10,410 10.70 1.74 -- 11/09 20M .70 .77 J(I2. .11 -- 1/M 7079 .84 ,78 9. HO .12 n/ce 7049 .87 .81 9. 29827. 42418. 4043. 50349. 57135. 48411. 3041. 3427. r.37. 5944J. 45114. 83298, 2473. 3072. 0. 57489. 439S0. 7939. re 11.410 .48 iw 71 .e .74 10T. 2SI4. 2940. 0. 1404S. 13370. 18171. re re 9.950 9.* -- 1W 21 .75 .81 99. 11.CAO IO .34 11/05 27)0 .83 .77 94. 434. 84734. 28352. 2072J. =3/14. 7)324. 2819. 31. 0. 20721. rjfffR. 79A28. re 10.400 .44 1U05 72 .81 .63 107. re 1U10 1.53 -- 11/ 7251 .78 .84 115. re tua .13 11/(0 P II .71 .78 122. 231. 4449, 3190. 5494. 0. 3379. 14740. P790. 17274. 6725, 2it1U01Z3t,. 3100. (ffl. 6. 79913. 70151. 904JI, re re re re 10.370 .1* -- 11/(0 2231 .74 .79 104. 11.440 <0 10.9 re .09 IH 0158 .83 .80 110. .04 U/S CI8 0. .80 110. 11.SM .91 -- 11/05 0739 .72 .78 1. 270. 4443. 2474. 75712. 78S72. 99430. 2144. 99. 0. 21. 0, 0. U44J3S504.. 45753. 4575?.. 82*95. ?*. * 19078. 24403. 8419. 57525. 40593. 77400. re re re re re re 11.5 10.PO 10.130 10.300 ll.OM 1C.010 .74 IH 0=9 .77 .78 1(3. .47 -- U/M 0319 .81 .79 104, 1(1.34 -- ll/ce 04 .75 .79 m. re .47 U/M CAB .47 .74 97. re 70,9 11/05 0445 0.00 .81 147. re .CO 1WCS 0505 1H4 .78 110. 1932!, 71090. 8327. 49985. 777S7. 93277. 10411, noe. 54. 47*12. 48351, 87047. 2*<nro, 37MT0, 9249;. 75=3. 7X41, 92431. 78. 0. 7535. 340.19. 0. 34. mtO. 2997. 24431. 27. W I. 274S. Vf 0. 0. 0, 71800. 49795. 89419. I ' s n e i TEt n s o r n i s e l i * m T M TO is s t m t t .o cf h/e 3 a i trri caxcr i i is t t f atur. ot i f t p t e aare i x z ftic r a r cf K ip t u p a ff fSiCW3mwc PtfiCtTTli SCM 8^Pate * w ; a z x p c p waF-jw^ctcns.w FW ie ji *.a * t o t s p iees XiTrrCTED i -detectiw unit .Atti) r F.EWWTCTO I - Tj< ^ ^ "X . 'i -. _ ; > V SU5JSCT ro PROTECTIVE O RDER. C 1 0 9 2 4 Onno^ N EVO AND UN DERSTO O D * Y DATE SUBJECT JO B NO. 7 io .( f. U l TI W I W n P R E P A R E D BY (S IG N A T U R E ) N? 2637232 date TOT WT BTOT msisiTOgip, ntr:mLAOMTarr T A t t t C l - r ) <X C lK : M ftT lft .721 jarsiTi .t:* sa r j s r f s ---- KTSf M KTTRS t t f *TB) *0 L ktrc :*. * : m 1'.? U'.TRfi II? H W l 113 NITRO 113 F ! rrm WW j j j j .) j j j j OEM r ft io n SC 10.135 K 1D.M SC 10.300 K 10.570 t t 9. RM K 9. R SC 10.9*0 SC 10.500 SC 10.000 PPT TOT .L s SCYTjrJX 3 333 l T f Tltc 333 331 .SI a 1.73 3.70 .ST tt.ZJ .33 .33 -- un un -- un -- un -- un -- un -- un -- un .07 u n U3l 12 1513 1533 ITO 1U5 Itft 1737 1717 .3 HH .T* .71 .87 .7* .1 .40 HH .75 103. SI 177. .74 78. .75 N , .87 113. .73 98. 83 108. .87 108. .n ica. 330 1377. 0. 3CS3. *81*1. sa*. 33*10. 3 l. 1814. 0. 333 lu s. 0. 488. 47*. 9*37. 27318. 3030. 7451. 0. TSI irai. 0. itn . = 7*. 4*70. r.w . 2413. 27*3, 0. 79* -- ru , T. 7481. 3371*. 77140. BU, 27VS3. 7770. 27747, 332 -- SUS. m *. *030. U18I. 31(87. 7104. 3399^. W 57. 32990, XX --. 4840. 2498. 1 BIS. ` WE77. 3831*. 9109. *135. 3577*. *17*8. I CaREKEB FCP CDCSlS^ON V t W TOT ISJPMCT .007 DF N/E 321) TTCT5ESI r: ISCT.T Ratto CCT CF TP TW .E w e e Ti I K C a.T (F TITTeaE E ia 5<*<Tff.t* PrfilttOL STM S*3frbiTmew* PQUTRCP MP.CKflWBi*) Ft-HELD BLMK L.mtHWE T O 9WS K*GT DHTCTED I.KHiEteTOt LiniT F IL P i TOTC4 G i i r i ^ N T I A L Cl 0925 SU B JEC T TO PROTECTiVE ORDER. Onnoo H S AO ANO U N Q C M T O O D Y D A TE j e '-- r cc S ffc- ''e> . , if'C" ^ Anilyjt -o=c C<>* ir-' S _& *s - -c - o -e0iJC'W'Cvl >i -- _C4 'J C is . o* J :a ^ sj ^ V a b _-c vc> -J1 --o o(1 n N V 0 lv - 2: -* J H - 0 J v L,i V *r c-i; J ? ZC'&ifr-j- 2>> Volume (nl) c 2n3--* <r 4>\A ^" ^w w^ Os. ^^ SUI J . * tr. _ -$ Ui'i $ !i j J l ----------- S - J ^ S Bottle Kunber y r \ >J"N V :\ 0 r> j .-- - -I .. . A J L SUBJECT TO PROTECTIVE ORDER 00023 C10926 ^0 B I4? ? ** ____ ^' >^C* *~ n0 a n 53 CX * o ~ff~ * 3 4 as y m I i a> t"o -H > N Si *3 2 ?93 C.1 6 ri Su b je c t ____________ __________________________ Da t e _________________________________ _ u ______ read And Understood Dy Me i i SUBJfCT__________________ 1___________________ Da t e __________________________________n _______ RCAO AHU UHDf RSIOOD BV HL a. * ~\ o -c t t --\ Anj1ys t > * \7"- 3" . r- r d S ^3 n -* 2J>L J) Ji J i '*s~rf -J ^ ^V S sv a i^1 -*1 ^^vNJa c* V ^&1 ^ -- 0 ^ Kfi J -i ? (-'*. V0 .c N ' ^ M L ' I " A -so oVw Voliera (ul) o3 -c< V v M -C ^ -X -J ^ -, .5 Botti* Nirntwr 5n o n o w *H f C10928 / 7 vi V -24 >o o .S Bottle Number > 3 9 O cor a L'i li J. SU BJECT TO PROTECTIVE O R D ER C10929 NIAHTO R lIK A R C H CORPORATION DAYTON LABORATORY SUBJECT JOB NO. \1 / ^ LsJ V I I Pa t T' Si gnature____ -1_ \ il. j*-kr* --- -- -- -- - ~ -- ... .1 '32i n J ` 0_ 0 $ -- -- 7 0 ? M i L. <PP ta 5 / PZ/.`>t j . i i 1 -A oh / j * '/J-L-- M T.Lv o t 2* *r . l ( iy .H h t v ooix. p s 1 7 ^1 I0 -- y / fr * ,1 '/is f a *T- --. r# / OlWl f t n*>.- . ----, !-- -- -- - -- - ?Mi *--- - -- -- ---- -- -> !HH r ___ ? k -- ---- - .. - - . fi - - xjb ini' IjOHi iS m iiA 19 R E A D A n d u n d e r s t o o d b y m e D a t e _____________ __________________ O iffa A J1 I V H M A A N L H W M r U K A T I U f l DAVTOtt LABORATORY JOB NO. Sig n a t u r e 1 I ----------------------- a T ira 7920 > Job Hat o f CRN A R . D i s c N uaber T ir a Day Pack 5 rat 5O wA S ta p le Id e n tific a tio n ifof t> 3 f , _ J _______ f r A a . Q < ^ 1 a n ^ lik U ` V ** - IfL . Cf <L J c L . M t ---------. O il id i) rr jr O -3 _L 03 oi A 2- 3 4 / 0 . A A 1/ j o f' f l r - 3 Q i| 7 J t< l iflO J i/* Sa 1 a * < r roi tf T- 50<J > rti*K ' r i * m 7 2- U j/.J 4 ? D< 0 /jL fl f* J ; r>,v m i 2LmS L J x U Q l P A f r tv oT l M ?^o ^Tu 1~ P f \ C 'K f " r o . C r t - O m 1 /AiiXf ' ^ c r \ ? . ,, L c ~ v r ? n - <'1 T /1 x so t i t i r < ? 3 / HLfl_ r/ T C P Er J t jiML " / / o . T i ^ ) P C ( r > p ( * f / o X i 3--r------ o < 3aj Da t e C osm ents # 7 ? -J 0 U w 1 . 1 i r 1, w ------- > ~nk- j o n> wH- r w /: o ------- i ' / p p J x A I i T * *V o 119 A lS B o t t le I Number | OC C o n d i t i o n s Run T ira /I ^ /2 _ A fri 7 d VI V 77 7f 7 //I tH co Ci o i Xr *7>---- V' **< n / 1 \ \ n ^ - > / < A O D T c x 1 - \ /l' `T i ^ r - / / / o / OO , -2 iio - i/iA - - r f "2-^ -j 4 T~ - i o [/ II /O .ff Ci co O o ! 4 io O O CO CO CO e< V IT . (Vi O a-, I iV i f ro d1 io Q *3 io \ -U CO \ IO (O TJ IO (.0 C3O IO <a3 i (-* \ <o \ io tn G> <r> C r? I0 3 i 5 H J cs Ci r "l V > a> j O O V <r> ro Gi O G< O G* G'-* _-* i*-i G c< G Cf _u_ 1 i 1 * 1 Ci es - fit os --H *- G'_ >7 . en i OS CO .- IO CT' OS- dp1 c 10 en * S * / S t ' 1/ZQQ I * n n s ' nure 9 * 1 3 Q ' S Z / Z / l - Q Q Z %ZZZ-dZ -- ro O Gi 10 \ h ro ^ cn-j ro os_ 0~>n G) ro os co - O to. ro en o G ^ s -- s ro en CS TO1 H U1_ o G C> MS d a t a f i l e h e a d e r f r o m >G010 S- am p 1e i i'U L 10 0 2 / 4 3 / * 2 S O p e r a t o r ! GARY MS 2 ll/ 0 9 / 3 4 '' 1 3 f 5 1 -' M is e : P 2 3 3 2 0 0 - 1 / 3 / 2 5 0 GT BTL*03 BTL# 3 S y s . ft: 1 MS m o d e l : 8 7 S1J/HW r e v . : CA A L S ft : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 Ho. o f e x t r a r e c o r d s : 2 Source te m p .: 250 A n a ly z e r tem p .: 265 T ra n s fe r lin e temp. : 2 6 5 ...,- .. Chrom a to g ra p h i c t emperat u re s : 280. C hi r o ma t o g r a p h i c t H it'S,i m i n . : 1 . 0 C h r o ma t o g r a p hi i c r a t e . d e g / m i n : 3 . 0 250. 25.0 0 .0 0. 0 .0 0. 0 0. 0 .0 ' 0.0 0. 0 .0 0 .0 M/Z - 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak is t a n g e n t skimmed c o r r e c t ed a r e a . Peak ft R. T. fii i r~i. 1 10 . 754 10 . 754 M/Z = i"*1 . 9 f i rst s c an 163 163 max s c an 179 179 1a s l pe ak sc an w id th 195 27 195 27 raw area 100823 100328 co rr. area 65566 63716 c o rr. 'A 100.00 9 7 . 13 . F i r s t p e a k ii s b a s e l i n e drop c o rre c te d a re a . S e c o nd P e ak ii s t a n g e n t s k i m m e d c o r r e c t e d a r e a . Peak ft R. T. f i r s t mi n . sc an ma x s c an 1a s t pe ak s c an w id th raw area co rr. area co rr. ym 1 10 . 754 171 179 266 10 . 754 171 179 20 6 35 35 98202 98202 54452 52754 100.00 96. 83 332/334 CALCULATION R - G l o b a l C 0> = .8305 F i r s t p e ak i s b a s e 1 i n e d r o p c o r r e c t e d a r e a . S e c o nd p e a k i s t a n g e n t s k i mmed c o r r e c t e d a r e a Peak ft R. T. f i r s t mi n . scan max scan 1as t peak C, c a n u i d t hi r aw area 1 1 0 . 7 7 4 165 18G 196 31 3 5 2 3 3 2 1 0 . 7 7 4 165 180 196 31 8 5 2 3 8 M/Z = 3 2 1 . 9 F i r s t p e ak ii s b a s e l i n e drop cor r ee t ed area. S e c o n d p e ak i s t a n g e n t s k i rnni e d c o r r e c t e d ar- e a P e ak ft P. T. mi i*i , firs t scan 1 10.774 10.774 175 175 max s c an 130 ISO 1ast p e ak --c an w i d t hi 190 15 190 15 p n n P/i raw ar ea 31299 31299 con-. area cor r . i 46364 100.0O 43853 ` 34.58 c o rr. are a 12159 11611 corr. A 100.00 9 5 .4 9 Cl0934 SUBJECT TO PR O T C m V F ORDER M-'Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R .T . min. f i rst scan max scan 1a s t peak s c a n w i-d t h r au area 1=- 1 0 . 7 7 4 1 76 1 80 191 2 1 0 .7 7 4 176 180 191 15 2 8 0 1 3 15 2 8 0 1 3 ^ (^ o ii o co rr. area 8798 8588 c o rr. X 100.00 97.61 320^322 CALCULATION R - G lo b a K 1) = .7236 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tan g en t skimmed c o r r e c t e d a r e a . Peak 4 R .T . rni n . f i rst scan max sc an 1a s t scan peak w id th raw area 1 I O . 795 178 181 186 2 1 0 . 7 9 5 178 131 136 S 17155 3 17155 co rr. area 5723 5443 corr. 100.00 9 5 . 11 < 32 0 + 3 2 2 >s <3 3 2 + 3 3 4 ) C A L C U L A T I O N R-G1obal< 3) = .1746 <328')>'<332 + 334 ) CALCULATION R -G lo b aK 3) = .3854 Onmp CONFIDENTIAL SU BJECT TO PROTECTIVE ORDER. C10935 Ci L i) CM N CO \ I <9 Ovl CO CO CM L CO CM \ co t^ \ CM o 3 CM D ETT CO CO M> CO CM LO CM \ \ *-< I CO (M a</>. (M . \ 00 O\J Zi CM CM CO I CO co Ql iH b. <9 CD IO (M \ CO \ I CO <M CL 0 CM 0M0" (\M 3 CM D e ifl *fi 0) CM CO I I- CM CO li) a< u. F i l e >GO 1 1 3 2 1 . 6 - 3 2 2 . 6 a m u . S U L 1 . 8 0 2 / . 4 8 / . 2 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 s o> <3 til OJ \ CO I >3 Ol CO OJ l(iA. OJ \ CO ^r \ OJ CD 3 CO Oi 3 OJ E rK Ul OJ . ui r- ir* OJ OJ 1' OJ i3 <3 *3 l 41 HS d i t a f i l e h e a d e r f r o m : >G0161 S i m p l e : 2 U L 1'. 0 0 2 / . 4 8 / . 2 S O p e r a t o r : GARY MS2 1 1 / 0 9 / 8 4 - 1 4 i-J 1 M is e : P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL#05 BTL# 5 S y s . tt; 1 MS m o d e l : 87 SU/HW r e u . : Cfl AL S * : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 No. o f e x t r a r e c o r d s : 2 Source tem p .: 250 A n a ly ze r tem p.: 265 T ra n s fe r lin e temp, : 2 6 5 - - '- - Chroma to g rap h i c t ernperat u re s : 200. 250. 0. 0. 0. Chromatographi c tim e s, min. : 1.0 25.0 0 .0 0 .0 0 .0 Chrom ato g rap h i c r a t e , deg/m i n : 3 .0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s tan g en t skimmed c o r r e c te d a re a . Peak tt R. T. min. ft rst s c an max s c an 1a s t peak sc an w id th raw area co rr. area co rr. V. 1 1 1 .4 2 4 198 212 232 2 11.424 198 212 232 34 109186 34 109186 66788 62232 100.00 9 3 . 18 M/Z = 3 3 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . S e c o n d p e ak i s t a n g e n t s k i mrned c o r r e c t ed a r e a . Peak * R. T. min. f i rst s c an max s c an 1 1 peak sc an w id th raw area co rr. area co rr. * 1 11.424 2 11.424 198 212 198 212 235 235 37 10274 37 100274 56170 53247 100.00 9 4 .8 0 332/334 CALCULATION R-G1o b a l< 0) = .8410 M/Z = 3 2 7 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area . Se c o n d p e a k i s t a n g e n t s k i mrned c o r r e c t e d a r e a . Peak # R. T. min. fir s t sc an max sc an 1ast peak scan width raw area 1 1 1 .4 4 4 263 213 227 24 75197 2 11.444 203 213 227 24 75197 M/Z * 3 2 1 . 9 F i r s t pe ak i s b as e 1i n drop c o r r e c t e d an e a . Second peak i s t an g e n t skimmed c o r r e c t e d a re 'a. Peak # R.-T. min. f irst sc an ma x s c an 1a s t peak sc an w id th raw area 1 11.444 11.444 199 213 233 199 213 238 39 147338 39 147338 co rr. area 46205 43385 co rr. '4 10 . 0 0 93.90 co rr. area cor r . y. 9890 94142 160.00 9 5 . 19 C10937 s M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak * R. T. min. f i rst scan max sc an 1a s t peak sc an u i dt h raw area 1 .--11.444 201 213 229 2 1 1 .4 4 4 201 213 229 28 104678 28 104678 0 '^ ' co rr. area 71022 65394 corr. y. 100.00 92.08 320^322 CALCULATION R - G 1o b a l < 1) = .7181 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tan g en t skimmed c o r r e c te d a r e a . Peak * R . T . fi rst min . scan max scan 1as t peak scan width raw area 1 11.444 2 11.444 199 213 232 33 199 213 232 . 33 85860 85860 corr. area 40386 37746 corr. v. 100.00 9 3 .4 6 C320 + 322)/(332 +334> C A L C U L A T I O N R -G 1o b a l < 3> = 1.3820 (328'>/<332 + 334 ) CALCULATION R-Global( 3) = .3685 P nn35 i C10938 F i l e >&01 .b 4.6 amu 2 U L U T - 3 1 0 9 P 233 0 2 0 0 - 1 / 3 / 2 5 0 GT File >C016 321.6-332.6 amu.2UL T-31G9 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT F ile Tt 7 T SUBJECT TO PROTECTIVE ORDER. 0003 C10939 MS data file header from >G0162 Sam ple: 2UL UT-3109 O p e r a t o r : GARY MS2 11'09/84 Mi s c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL#07BTL# 7 S y s . #: 1 MS m o d e l 8 7 SU/HW r e v . : CA A L S # : a Method f i l e : SP2330 Tuning f i l e : APEI01 No. o f e x t r a r e c o r d s : Sourc e t emp. : 250 A n a l y z e r temp > 265 Tr< in s f e r l i n e t emp. : 14 : 3 i Chromtographi c t emperat ures : 200. 250. 0. 0. 0. Chromt, ograph i c t im e s , m in. : 1 .3 25.0 0 .0 0 .0 0 .0 Chrom atographi c r a t e , deg/m i n : 3 .0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Sec ond pe ak i s t an g ent skimmed c o r r e c t e d a r e a . Peak # R. T. min. fi rst sc an max scan la s t peak scan width raw area co rr. area c o rr. y. 1 11.462 2 11.462 210 210 214 214 219 219 9 20045 9 20045 6860 5717 100.00 83.34 M/Z = 3 3 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Sec ond peak i s t a n g e n t skimmed c o r r e c t e d a r e a . Peak # R. T. min. firs t sc an max scan 1a s t scan p e ak w id th raw area co rr. area c o rr. * 1 11.462 212 214 218 11.462 212 214 218 6 13497 6 13497 5115 100.00 4614 90.21 332^334 CALCULATION R - G 1o b a l < 0> = .7456 M/Z = 3 2 7 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak i s tan g en t skimmed c o r r e c te d a re a . *P e a k R.T. f i r s t min. sc an max sc an 1a s t peak sc an w id th raw area 1 11.482 212 215 219 2 11.482 212 215 219 7 1362 7 13620 M/Z = 3 2 1 . 9 F i r s t p e ak i s b a s e 1 i ne drop c o rre c te d area . Sec ond peak i s t ange nt skimmed c o r r e c t e d a r e a . Peak # R.T. f i r s t min. sc an max scan 1as t p e ak s c a n w i "d t h raw area 1 11.502 2 11.502 ---------- ------ ,, ------ 213 213 ------ 216 216 218 5 21 ? 5 OOC7 8075 8075 c o rr. area 4779 40S9 corr. * 108.00 8 5 .5 6 co rr. area 1665 1482 corr. ;/ 100.00 89.01 Cl0940 fl^Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Re ak 4 R. T. min. f i rst scan max scan 1a s t peak s c a n u i `dt h raw area 1 ' 1 1 .482 215 215 217 2 4026 2 11.482 215 215 217 2 4026 >& c i b 2_ c o rr. area 1372 1330 co rr. ;/ 100.00 9 6 .9 4 320/322 CALCULATION R - G lo b a l( 1) = .8240 M^Z = 2 5 7 . 0 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . S e c o n d p e a k i s t a n g e n t s k i mmed c o r r e c t e d a r e a . Peak R. T. min. fi rst sc an max sc an 1a s t peak scan width raw area 1 1 1 .4 6 2 213 214 214 2 1 1 .4 6 2 213 214 214 1 2961 1 2961 corr. area 1551 1430 c o rr. 100.00 95.42 (320 + 322)/(332 +334) C A L C U L A T I O N R-GlobalC 3 ) = . 2536 (328 ' ) / ( 3 3 2 + 334) CALCULATION R - G 1o b a l ( 3 ) = .3978 o o o r- .R ,-#***>.^.7 7 - 7* - -4 d SUBJECT TO PROTECTIVE ORDER, C10941 G G* Cl0943 F i l e >&O 6 3 3 3 3 . 6 ~ 3 3 4 . 6 aTiu.^'-^ U T - 3 1 1 0 Ti i \. *-* fO 'TV O T' *=' O' tO to O' 1 ro 10 O' (3l* C 10 1 (l> 3P235 t> ~n 1f.0i to O 10 M I O II -* \\ to to s\ ro io tn tn <n MS d a t a f i l e h e a d e r f rom > G 0 1 6 3 S imp 1e : 2UL i r r - 3 1 1 0 S O p e r a t o r : GARY MS2 11/09/84 14:52 M ise P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL09BTL# 9 S y s . #: 1 MS m o d e l 8.7 SW/HN r e u . : Cfi A L S # ; 0 Method f i l e : SP2330 T u n i ng f i l e : A P E I0 1 No. o f e x t r a re c o rd s : 2 S o u r c e t e m p . : 25 f i n a l y z e r t e m p . : 265 T ra n s f e r 1i ne temp. : 265 - Chromtographic tem peratures : 200. Chrom atographic tim e s, min. : 1.0 Chrom tograph i c r a t e , deg/m in : 3 .0 250. 25.0 0. 0 0. 0 .0 0 .0 0 0. 0 0. 0 0. 0. 0 0. 0 M/Z = 3 3 3 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s tangent skimmed c o r r e c t e d a r e a . Peak # R. T. mi n . f i rst scan max scan 1a st scan peak w id th raw area co rr. area c o rr. yt 1 11.583 218 228 222 2 11.583 213 220 222 4 9162 4 9162 2698 2662 100. 00 98. 67 M/Z = 3 3 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s tan g en t skimmed c o r r e c t e d a re a . Peak # R. T. min. f i rst s c an max sc an 1as t scan pe ak wi dt h raw area co rr. area c o rr. y. 1 11.583 2 11.583 218 218 220 220 221 221 3 6854 3 6854 2336 2079 100.00 89.00 3 3 2 / 3 3 4 C A L C U L A T I OH R - G l o b a K 0> - ,8659 M/Z = 3 2 7 . 9 F i r s t peak i s base! ine drop c o rre c te d area . Sec ond peak i s t ange nt skimmed c o r r e c t e d a r e a . Peak 4 R. T. min. f i rst sc an max scan 1a s t scan pe ak w id th raw area 1 1 1 .6 0 3 219 221 223 4 8023 2 1 1 . 6G3 219 221 223 4 8028 M/Z = 3 2 1 . 9 F i r s t peak i s b a s e ! i ne dro p c o r r e c t ed a r e a . Second pe ak i s t a n g e n t skimmed c o r r e c t e d a r e a . Peak # R. T. mi n . f ir st sc an max s c an 1a s t p e ak s c an w id th 0 raw area 1 0.000 2 0.000 224 224 0 0 C j / i ^ it '1 1AL' , : `v t cuts ir r r tc \ D o o T rrrn / r o o n tra 223 223 -1 -1 oon4n 0 0 c o rr. area 2356 2052 c o yr r . 100.00 87.10 corr. ar ea 1341 1341 co rr. 100.00 100.00 1 Cl0943 n/z - 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak * R. T. min. 1 -, 0 . 0 0 0 2 0.000 f irst scan 204 224 max sc an 0 0 1ast peak sc an u r dth 223 -1 223 -1 raw area 0 0 '=>C* I Lo 3 co rr, area 1345 1345 corr. * 180.00 100.00 320x322 CALCULATION R-Global< 1 ) = 1.0O30 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s ta n g e n t skimmed c o r r e c t e d a r e a . P e ak * R. T. min. firs t sc an max sc an 1ast peak scan width raw area 1 0.000 2 0.000 224 224 0 223 0 223 -1 -1 0 0 co rr. area 1605 1605 c o rr. v. 100.00 100.00 <320 + 3 2 2 )x ( 3 3 2 +334) CALCULATION R - u 1o b a l< 3) -- .5336 < 328')x< 332 + 334) CALCULATION R-Global< 3) = .4656 ~ : 2 J i 'J .. C10944 File >0164 4.6 amu.2UL UT-3111 SP2330 200-1^3/350 GT F i l e >63164 3 2 1 .6 - 3 2 2 .6 amu.SUL UT-3111 S P 2 3 3 0 2 0 6 - 1 / 3 / 2 5 0 GT GC/IIS d efu It file: >G01o4:;fl4 MS d a t a f i l e h e a d e r f r o m : >G0 1 64 Sam ple: 2UL U T - 3 1 U O p e r a t o r : GARY MS2 11/09/34 15:12 M is c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT B T L # 1 1 B T L # 11 S y s . #: 1 MS m o d e l : 8 7 SW/HU r e u . : CA A L S tt : 0 Method f i l e : SP2330 T u n in g f i 1e: APEI01 Mo. o f e x t r a r e c o r d s : 2 Source tem p .: 250 A n a ly z e r temp . : 265 T r a n s f er l in e temp. : 265 Chromat ograph i c te m p eratu res : 200. 250. 0. 0. 0 . Chr omato gr a p h lc t im e s , min. : 1 .0 2 5 .0 0.O 3 .0 0 .0 C hrom atographi c r a t e , deg/m i n : 3 .0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F ir- it peak i s b a s e lin e drop c o rre c te d area . Second peak i s tan g en t skimmed c o r r e c t e d a re a . Peak # R .T. min. firs t' scan max scan 1a s t peak sc an wi dt h raw area co rr. area c o rr. / 1 11.746 224 23 232 2 11.746 224 223 232 3 16531 3 16531 5315 4231 100.00 79.60 M/Z = 3 3 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d area . S e c o n d p e a k i s t a n g e n t s k i mmed c o r r e c t ed a r e a . Peak it R .T . mi n . 1 11.766 2 11.766 firs t scan 226 226 max scan 229 229 1a s t sc an **i 232 peak wi dt h 6 6 rau area 12233 12238 corr. area 4 030 3346 corr. X 100.00 83.03 332/334 CALCULATION R - G lo b a K 0? = . 7582 M/Z = 3 2 7 . 9 F i r s t peak i s b a s e lin e drop c o rrec ted ar ea . Sec ond peak i s ta n g e n t skimmed c o r r e c t e d a r ea. Peak tt R .T. min. firs t scan max sc an 1a s t peak sc an wi dt h raw area 1 11.737 223 230 232 2 11.7 37 223 238 232 4 8937 4 8937 M/Z = 3 2 1 . 9 F i r s t peak i s b ase ! i ne drop c o rre c te d area. S e c o n d p e ak i s t ari g e n t s kim m ed c o r r e c t e d a r e a . Pe ak tt R .T. mi n . f irst sc an max scan 1a s t pe ak sc an w id th raw area 1 11.737 227 230 233 6 10530 2 11.787 227 233 f 233 6 10530 ' Onn^ c o rr. are a 2765 2613 c o rr. area 2638 2370 co rr. 100.00 96.60 co rr. 100.00 8 8 . 17 C l 0946 M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. P t ak 41 R. T. min. r " 11.766 2 11.766 fi rst scan 228 223 m ax sc an c>? 9 229 1a st scan 233 233 peak w id th 5 5 raw area 8S33 8833 > C s oi u ?4 co rr. area 2053 1938 co rr. 'A 100.00 94.40 320/322 CALCULATION R - G l o b a K 1> = .7638 M/Z = 2 5 7 . 0 F irs t, peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tan g en t skimmed c o r r e c t e d a r e a . Peak 44 R. T. min. fi rst sc an max sc an 1a st scan peak w id th raw area 1 11.787 229 238 232 3 6677 2 11.787 229 23 232 3 6677 co rr. area 1913 1357 c o rr. mA 100.00 97-. 0 7 <320 + 322> /< 332 +334) CALCULATION R -G lo b aK 3) * .5073 < 3 2 8')/< 3 32 + 334) CALCULATION R - G l o b a K 3> = .2869 \ n o 'M A v ! * SUBJECT TO PRCTcCTIVE ORDER. C10947 SP2336 266-1/3/250 <o tn CO in i\J \ ro \ p4 I co OJ C01O OJ CL am u.2U L U T-311`2 *r i't o 3 OJ D e *T> '> OJ 01 CIO Jj 01 U1 o Ci 0 l i ) LO OJ OI OI \ \\ O) 0) O) \\ 1II 0 0o 0IT* 01 OJ 01 0 Cl 0 CO 0) co co- (0 co 01 01 01 Cl O) CO)L OI CO I 3 OJ OI OI o cOoJ LO O CJ* /S 1> 01 01 O) I OI D t=1 0 01 co I 'O a* co IO *! co I 3 OJ D O) ON fLO OI r-Iw 'O LO OJ LO Ci IO A ao a> o iH O ITi o- C C- c MS data file header from >G015 Saffi p i e 2 U L U T - 3 1 12 O p e r a t o r : GRRY MS2 11/09/84 15:32 Mi s c S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL#13BTL#13 Sys. # 1 MS m o d e l : 8 7 SW/HU r e v . : Cfl R L S # : 0 Method f i l e : SP2330 Tuning f i l e : RPEI01 No. o f e x t r a r e c o r d s : 2 Source te m p .: 250 A n a ly z e r temp. : 265 T r a n s f e r l i n e t e m p ,> : 2 6 5 ............ ' C h r o mat. o g r a p h i c t e m p e r a t u r e s : 2 0 0 . 250. 0. 0. 0. Chrom itographi c tim e s, min. : 1.0 2 5 .0 0 .0 0 .0 0 .0 Chrom atographi c r a t e , deg/m i n : 3 .0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak i s tan g e n t skimmed c o r r e c t e d a re a . Peak * R. T. min. f irst scan max scan 1a st peak scan width raw area co rr. area c o rr. `4 1 11.913 2 11.913 230 230 235 235 246 246 16 81281 16 81281 5S577 53057 100.00 90.58 M/Z = 3 3 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s tangent skimmed c o rre c te d a re a . Peak # R. T. mi n . firs t scan ma x scan 1a s t peak sc an w id t h ' raw area corr. area co rr. * 1 11.933 228 236 243 2 11.933 223 236 243 15' 64 086 15 6 4 0 8 6 44181 34348 100.00 77.74 3 3 2 / 3 3 4 C R L C U L R T I ON R-G lobaU 0) = . 7542 M/Z = 3 2 7 , 9 F irst, peak is b a s e lin e drop c o rre c te d area. Second peak is tangen t skimmed c o rre c te d a re a . Peak R. T. f i r s t max 1a s t peak # min. scan s c an . sc a n w id th raw area 1 1 1 .9 3 3 228 236 241 2 1 1 .9 3 3 228 236 241 13 5 3 9 5 3 13 5 3 9 5 3 M/Z = 3 2 1 . 9 F i r s t peak i s b as e 1 i ne drop c o rre c te d area . Sec ond pe ak i s t a n g e n t skimmed c o r r e c t e d a r e a . Pe ak # R. T. min. firs tscan max sc an 1a s t peak sc an w id t h raw area 1 11.953 229 237 _ .2____11--9 5 3 --- -2 2-9 m ^' . i a i , SUBJECT. TO PROTECTIVE ORDER. 2 47 18 247 18 pnn^g 92820 92820 c o rr. area 33322 22363 , co rr. area 67584 58962 cor r . '4 100.00 6 7 . 11 corr. '4 100.00 87.24 C10949 > M/Z = 3 1 8 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area , Second peak is tangent skimmed c o rre c te d a re a . F'e ak # R. T. min. firs t scan max scan la s t scan peak w id th raw area 1 -11.953 2 11.953 229 229 237237 244 244 15 68471 15 6 S471 > r 0 l i i ? 5 co rr. area 43191 37301 corn, *4 160.00 77.46 320/322 CALCULATION R - G lo b a l< 1) = .7131 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak is t angent skimmed c o r r e c te d a re a . Peak (t R .T. min. f i rst scan max sc an 1a s t peak sc an w id th raw area 1 1 1 .9 5 3 233 237 241 2 1 1 .9 5 3 233 237 241 8 36664 8 36664 co rr. area 22728 17964 c o rr, v. 160.66 79.64 ( 3 2 0 + 3 2 2 ? / C3 3 2 + 3 3 4 ) C A L C U L A T I O N R - G 1o b a l ( 3 ) = 1. 1267 ( 323 / ) s (332 + 334) CALCULATION R-Glob&l< 3 > - .3184 \i C10950 File > Glte- 33 e-- 3 J4 t' clmu SUL UT-3113 SP2330 200-1/3/256 GT F i l e >G0 1 6 321 . 6 - 3 2 2 . 6 - am u. SUL U T -3 1 1 3 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT rf - ...... .. \ T PROTECTIVE ORDER- SUBJECT TO < in o 4 R C10951 GC/MS default file: >CG166::A4 MS data file header from : >G0166 Sam ple: 2UL UT-3113 O p e r a t o r : GARY MS2 11/03/34 15:53 M is c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT E T L # 15 B T L # 15 S y s . #: I M S mode 1 : 8 7 SW/HM r e v . : CA R L S * : 0 Method f i l e : SP2330 Tuning f i le : APEI01 Sourc e temp. : 250 A n a ly z e r tem p .: 265 N T o. ra n o s f f e e r x t 1 r i a n e r e t c e o m rd p ,i s :m 2 6 5 ............ T - Chromtographi c tem peratures : 200. 250. 0. 0. 0. Chrom atograph!c tim e s, min. : 1.0 25.0 0 .0 0 .0 0 .0 Chromt ograph i c r a t e , deg/m in: 3 .0 0. 0 0 .0 0 .0 0 .0 M/2 = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s tan g e n t skimmed c o r r e c te d a re a . Peak * R. T. min. f irst scan max scan 1a s t peak scan width raw area c o rr. area corr. vm 1 1 1 .8 0 4 225 231 236 11 5 8 4 0 2 38316 100.00 1 1 .8 8 4 225 231 236 11 5 8 4 0 2 31276 8 1 .6 3 M/2 = 3 3 1 . 9 F i r s t p e a k ii s b s e 1 i n e drop c o rre c te d ar ea S e c o nd p e a k ii s t a n g e n t s k i m m e d c o r r e c t e d a r e a . P e ak # R. T. min. f irst sc an max sc an 1a st peak scan width raw area co rr. area co rr. *A 1 11.825 2 11.825 227 227 232 *0*A1 236 236 9 46526 9 46526 31487 26010 100.00 82.61 332/334 CALCULATION R -G lo b al< 0) - . 3213 M/2 = 3 2 7 . 9 F i r s t peak i b a s e lin e drop c o rre c te d are a , Sec ond pe ak i t a n g e n t skimmed c o r r e c t e d a r e a . ik R . T . f i r s t max 1a st peak min. sc an sc an sc an w id t h raw area 1 11.845 2 11.845 227 227 233 o-TioO 239 239 12 4 7 2 0 9 12 4 7 2 0 9 M/2 = 3 2 1 .9 F i r s t peak i s b a s e lin e drop c o rre c te d area, Second peak i s tangen t skimmed c o rre c te d a re a . P e ak * R. T. rni n . firs t sc an max sc an 1a s t pe ak sc an w id th raw area 1 11.345 230 233 236 6 28150 2 11.845 230 233*. j_ . 2 3 6 6 20150 O nn^ V. Co r r . area 29245 25381 corr. * 16 0 .8 8 8 6 .7 9 corr. ar ea 9422 8732 core. * 108.80 92.68 C10952 s M/Z = 3 1 9 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak is tangent skimmed c o r r e c te d a re a . P e ak # R. T. min. l ' l l . 845 2 11 . S 4 5 f i rst scan 230 230 ma x scan 233 233 1a s t peak s c a n ui i d t h 235 235 5 5 rau area 18949 13949 ( j /i (> co rr. area 8174 6364 corr. yt 100.00 77.86 320/322 CALCULAT I ON R - u 1o b a l ( 1 ) = . 8 &7 5 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d area. Second peak i s tan g en t skimmed c o r r e c t e d a r e a . P e ak # R .T . mi n . f i rst scan max s c an 1a s t peak sc an u i dt h rau area 1 11.845 230 233 236 2 11.345 230 233 236 6 30162 6 30162 corr. area 6420 6324 c o rr. % 100.00 98.50 ( 3 2 0 + '322)/(332 +334) C A L C U L A T I O N R - G l o b a l < 3> = .2521 ( 3 2 8 0 / ( 3 3 2 + 334) CALCULATION R - G 1oba 1( 3 ) = .4177 S U B JE C T TO PrvOTECT'/E oRDEt 00^ 0 C10953 File > G 0 16 7 333.6-334.6 amu UL 10.02/.43^.20 SP2230 200- 1/3 / 25 0 GT.. F i l e >G0167 5 2 1 . 6 - 3 2 2 . 6 am u.2UL I D . 0 2 / . 4 S / . 2 0 S P 2 2 3 0 2 0 0 - 1 / 3 / 2 5 0 GT nnriS1. C10954 MS data file- header from > G0167 S a m p le : 2UL 10 . 0 2 / .. 4 8 / . 20 O p e r a t o r : GARY MS2 11 / 0 9 / 8 4 - 1 6 r M M is c : S P 2 2 3 0 2 0 9 - 1 / 3 / 2 5 0 GT BTL#17BTL#17 Sys. #: 1 MS m o d e l : 8 7 SW/HW r e u . : CA A L S # : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 No. o f e x t r a r e c o r d s : 2 Source tem p.: 250 A n a ly z e r tem p .: 265 T r a n s fe r lin e temp. : 265--*'-* . Chromatographic t em peratures : 206. 250. 0. 0. 0. ' Chromatographic tim e s, min. : 1.0 25.0 0 .0 0 .0 0 .0 C h r o ma t o g r a p h i c r a t e , d e g / m i n : 3 . 0 0 . 0 0 . 0 0 . 0 0 . 0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . S e c o n d p e a k i s t a n g e n t s k i fri med c o r r e c t e d a r e a . Peak # R .T. min. firs t scan max sc an 1a s t peak scan width raw area corr. area c o rr. * 1 11.260 2 11.260 194 262 210 194 262 210 16 96032 16 9 0032 68336 60928 100.00 89.16 M/Z = 3 3 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Sec ond peak i s t an gent skimmed c o r r e c t e d a r e a . Pe ak # R .T. min. f i rst scan ma x scan 1 t* p e a k sc an w id t h raw area co rr. area c o rr. y. 1 11.260 2 11.260 196 202 211 196 202 211 15 75797 15 7 5 7 9 7 56597 51129 100.00 90.34 332/334 CALCULATION R - G l o b a l < 0> = .8232 M/ 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . S e c o n d pe ak i s t a n g e n t s k im m ed c o r r e c t e d a r e a . Peak # R .T. min. fi rst sc an max s c an 1a s t peak scan width raw area corr. area 1 11.286 2 11.280 198 263 211 193 203 211 13 76469 58451 13 7 6 4 6 9 53459 M/Z = 3 2 1 . 9 F i r s t p e ak i s b a s e l i n e drop c o rre c te d a re a . Sec ond peak i s t a n g e n t skimmed c o r r e c t e d a r e a . Peak R .T . mi n . f irst sc an max s c an 1a s t pe ak scan width raw area co rr. area 1 11.286 2 11.280 192 263 212 192 203 212 29 1085361 157321 20 1085361 926731 SUBJECT TO PROTECTIVE ORDER. o n n 5 '! c o rr. 100.60 9 1 .4 6 co rr. y, 108.60 87. 65 C10955 tU Z = 3 1 ? . 9 F i r s t pe ak i s b a s e 1 i ne drop c o rre c te d a re a . Se c end peak i s t a n g e n t skim m ed c o r r e c t e d a r e a . Peak # R. T. min. fi rst scan max sc an 1a s t peak sc an w id th raw area 1 / 11.300 2 11.300 135 204 212 195 04 212 17 8 8 0 0 1 0 17 8 0 0 0 1 0 > C r O I (> H co rr. area 776953 695145 c o rr. >: 100.00 8 9 .4 7 3 2 0 / 3 2 2 C f l L C U L f t T I ON R - G l o b a K 1> = .7348 M/Z = 5 7 . 6 F i r s t peak i s b a s e 1 i nt' d ro p c o r r e c t e d a r e a . Second peak i s t angent skimmed c o rre c te d a re a . JO --1 Peak # min. fi rst sc an m ax sc an 1a s t peak sc an w id th raw area 1 11.300 2 1 1 .300 192 192 204 204 212 212 20 . ' 20 451265 451265 c o rr. area 416825 363455 c o rr, * 100.00 87.20 C3 2 0 + 3 2 2 ) / ( 3 3 2 +3 3 4 > C L C U L T I OH R - G 1o b a 1< 3 > = 14.6821 <3 2 3 ' ) / < 3 3 2 + 3 3 4 > C A L C U L A T I O N R -G lo b aK 3) = .3917 f ^z `-Ss i n o ^ r' C10956 Tile >G01 68 333.6-334.6 mu.2UL UT-3114 SF2330 260-1/3/250 QT F i l e >G0 1 6 S :21 . 6 - 3 2 2 . 6 amu . S U L - U T - 3 1 1 4 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT a *r * . L r > L , -j s L ^ L SU BJECT TO PROTECTIVE ORDER. T in /A f j C10957 MS data file header from >G0168 Sam ple: 2UL UT-3114 O p e r a t o r : GRY MS2 11/09/84 M i s e : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT B T L * 19 B T L # 19 S y s . #: 1 MS mode 1 : 3 7 . SU/HW r e v . : CA A L S # : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 No. o f e x t r a r e c o r d s : S o u rce ternp. : 250 A n a ly z e r ternp.': 265 Tran s f er lin e temp. * 1 6 :3 5 . -__C h r o m a t o g r a p h i c t e m p e r a t u r e s : 2 0 0 . * Chromatographi c tim e s, min. : 1.0 Chromatographi c ra te , deg/min: 3 .0 250. 25.0 0 .6 0. 0. 0 0 .0 0. 0 .0 0 .0 0. 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s ta n g e n t skimmed c o r r e c t e d a r e a . Peak # R. T. min. fi rst sc an ma x scan 1a s t peak scan width raw area co rr. area corr. V. 1 12.164 24 245 250 IS 23759 1 2 .1 0 4 240 245 250 10 2 3759 9109 6349 100.00 69.70 M/Z = 3 3 1 . 9 F i r s t pe ak i s b a s e l in e drop c o rre c te d a re a . S e c o n d p e ak i s t ari g e n t s k i mme d c o r r e c t e d a r e a . Peak # R. T. min. f i rst s c an 1 12.104 12. 104 242 242 max scan 245 245 1as t peak sc an w id t h 250 8 250 3 raw area 18562 18562 co rr. area 7106 5590 co rr, 5 100,00 78.67 332/334 CALCULATION R - G 1 o b a l < 0> = .7801 M/Z = 3 2 7 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak is ta n g e rt skimmed c o r r e c t e d a re a . Peak # R. T. min. fi rst scan max sc an 1a s t peak scan width raw area 1 12.124 243 246 250 2 12. 124 243 246 250 7 16139 7 16139 M/Z = 3 2 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s ta n g e n t skimmed c o r r e c t e d a r e a . P e ak it R. T. min. f i rst sc an max s c an 1a s t pe ak sc an w id th raw area 1 12.124 2 12.124 246 . 240 24 6 246 255 255 1, ti,.. r w `---i. i r . . ^ j_____ _ 1 ----- L./V 15 5 0 2 7 3 15 5 0 2 7 3 t/U W 'i c o rr. area 6108 5044 c o rr. ym 100.00 82.58 co rr. ar ea 29318 2384 0 corr. yt 100.00 79.61 C10958 s M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak * R. T. min. fi rst scan max scan 1a s t peak scan width raw area 1 v 12.124 2 12.124 241 . 241 246 246 254 254 13 4 3223 13 43223 > L o i g > ? co rr. area 22410 13094 co rr. * 100.00 80. 74 320/322 CALCULATION R - G 1o b a l < 1) = .7644 M/Z = 2 5 7 .0 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak is tangen t skimmed c o rre c te d a re a . R. T. min. F i rst sc an max sc an 1a st peak sc an w id th raw area 12.124 242 246 252 12.124 242 246 252 10 3 3 5 3 9 10 3 3 5 3 9 corr. area 11939 9289 co rr. y. 100.00 7 7 .8 0 ( 3 2 0 + 3 2 2 ) / <3 3 2 + 3 3 4 ) C A L C U L A T I O N R -G lo b al< 3) = 3.1901 (3 2 8 ' ) / (332 + 334) CALCULATION R - G 1o b a l ( 3 ) -- .3604 . ------ 7 r : _ ^ '4 -- r ) SU BJECT TO PROTECTIVE O R D E R o n n r^ C10959 Tile K-0165 ^ 7 34. amu.SUL. UT-3115 P2338 200-1 /3-'250 T F i l e > 9 0 1 6 9 3 2 1 . 6 - 3 2 2 . 6 amu . - 1->1lL. U I 1 ;:P 2 33 0 2 O 0 - 1 / 3 / 2 5 0 GT rin n f^ i* vL '* C10960 GC/MS default file: >G0169::A4 MS data file header from : >G0169 San.pl e : 2UL UT-3115 O p e r a t o r : GARY MS2 11/09/84 16:52 M ise : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 GT BTL#21BTL#21 S v s . <1: 1 MS m o d e l : 87 S U/ H N r e v . : CR A L S # : 0 Method f i l e : SP2330 T u n i n g f i l e APE I 01 No. o f e x t r a r e c o r d S ! 2 Source tem p.: 250 A n a ly se r temp. 265 T r ar. s f e r l i n e t e m p . ! tm65 * Chrornat ograph i c t e m p e ra tu re s : 200. Chrornat ograph i c t im e s , m in. : 1 . 0 Chrornatographi c ra te , deg/min: 3. 0 250. 25.0 0. 0 0. 0 .0 0. 0 0. 0 .0 0 .0 0. 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tangen t skimmed c o r r e c t e d a r e a . Peak R. T. min. f irst sc an max scan 1as t peak sc an w id th raw area c o rr. area corr. 1 12.244 245 250 257 2 12.244 245 250 257 12 6 3 7 2 5 12 6 3 7 2 5 41333 37763 100.00 9 1 .3 6 M/Z = 3 3 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d area. Second peak is tan g en t skimmed c o r r e c t e d a re a . Peak # R. T. min. fi rst sc an max sc an 1a s t pe ak scan width raw area c o rr. area c o rr. * 1 12.244 12.244 246 246 250 * 256 25 256 10 5 4 3 7 6 10 5 4 3 7 6 33996 31331 100.00 92.16 332/334 CALCULATION R-G lobaK 0) = .8225 M/Z 27.9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s tan g en t skimmed c o r r e c t e d a r e a . Pe ak # R. T. min. f i rst scan max scan* 1a s t p e ak sc an wi dt h r aw area 1 1 2 .2 6 4 246 251 257 2 1 2 .2 6 4 246 251 257 11 4 6 6 0 9 11 4 6 6 0 9 M/Z = 3 2 1 . 9 F i r s t peak i s b a s e lin e d r op c o r r e c t e d a r e a . Second peak i s t ange nt skimmed c o r r e c te d a re a . Peak * R. T. f i r s t mi n . scan max sc an 1a s t peak sc an w id th raw area 1 1 2 .2 6 4 247 251 255 2 1 2 .2 6 4 247 251 255 8 13966 3 13966 I ics i r r *-*'* corr. area 30010 26446 corr. '4- 100.00 8 3 . 12 c orr7 area 3030 2726 c o rr. y. 160.00 89.97 Cl0961 s M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak tt R. T. min. f i rst scan max scan 1a s t peak sc an w id th raw area 1 .1 2 .2 6 4 258 51 253 3 7490 2 '12.264 25G 251 253 3 7490 Qr \Le ^ co rr, area 2051 1985 c o rr. * 100.00 _ 96.78 320x322 CALCULATION R- G lo b a li 1) = .6769 MxZ = 2 5 7 . 0 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak is tangen t skimmed c o rre c te d a re a . Peak # R. T. min. f i rst sc an ma x s c an 1a s t scan peak w id th raw area 1 1 2 .2 6 4 250 251 252 2 7371 1 2.264 250 251 252 2 7371 c o rr. area 2613 2512 corr. Ji 100.00 9 6 . 13 #-- i 320 + 322>x<332 +334) CALCULATION R --G l o b a l i 3 ) = . y6f5 <328')x< 332 + 334 ) CALCULATION R-GlobalC 3) = .3988 :r X nr> o * C10962 F i l e >60170 3 3 3 .6 - 3 3 4 .6 *ffiu.2UL UT-3116 P2330 200-1/3/25 6T F i l e >60170 3 2 1 .6 - 3 2 2 .6 amu.SUL UT-3116 SF`2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 6 T CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. nnr\ C10963 MS data file header from : >G0170 Sam ple: 2UL UT-3116 O p e r a t o r : GARY MS2 1 1 / 0 9 / 8 4 1 7 : 17. M i s c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL#23BTL#23 Sys. #: 1 MS m o d e l : 8 7 SU/HW r e v . : CA A L S # : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 No. o f e x t r a r e c o r d s : 2 Source tem p .: 250 A n alyze r tem p.: 265 T r a n s fe r lin e temp. : 265--*'- !C h r orni a t o g r a p h i c t e m p e r a t u r e s : 2 0 0 . 2 5 0 . 0 . 0 . 0 . C h r o ma t o g r a p h i c t i m e s , m i n . : 1 . 0 2 5 .0 0 .0 0 .0 0 .0 Chi r o mat o g r a p h i c r a t e , d e g / m i n : 3 . 0 0 . 0 0 . 0 0 . 0 0 . 0 M/ Z = 3 3 3 . 9 F i r s t pe ak i s bas e l i ne drop c o rre c te d a re a . S e c ond p e ak i s t a n g e n t s k i mmed c o r r ec t e d a r e a . Peak * R. T. min. fi rst sc an max s c an 1a s t peak sc an w id t h raw area corr. area c o rr, y 1 1 2 .3 1 0 251 256 261 2 1 2 .3 1 0 251 256 261 10 5 47 0 8 10 5 4 7 0 8 4 1748 36103 100.00 86.48 M/Z = 3 3 1 . 9 F i r s t peak i s base 1i ne drop c o r r e c t e d a r e a . S e c o n d 1? e' ak i s t a n g e n t s k i mmed c o r r e c t ed a r e a . Peak # R. T. mi n . fi rst scan ma x s c an 1a s t peak sc an w id th raw area c o rr. area co rr. * 1 1 2 .3 1 0 251 256 261 *> 1 2 . 3 1 0 2 51 2 5 6 2 61 10 45680 32990 100.00 10 4 5 6 8 0 28725 87.07 332/334 CALCULATION R - G 1o b a l < 0> = .7902 M/Z = 3 2 7 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tangen t skimmed c o r r e c te d a r e a . Peak # R. T. rni n . firs t s c an max s c an 1a s t scan peak w id th raw ar ea 1 12.330 2 12.330 247 247 257 257 261 261 14 4 8 8 6 3 14 4 8 S 6 3 M/Z = 3 2 1 . 9 F i r s t peak i s b a s e 1 i ne drop c o rre c te d ar ea . Sec ond peak i s t angent skimmed c o r r e c t e d a r e a . P e ak # R. T. rii i n . firs t sc an ma x s c an 1a s t pe ak sc an w id t h raw area 1 0.600 262 _ . 0 . 0 0 0 2 6 2 SUBJECT TO p p n x p r^ iv c : 0 261 0 261 -1 -1 nnr\ 6 .1. 0 0 co rr. ar ea 29767 23483 c o yr r . 10 0 .0 0 7 8 . 91 co rr. area 1273 1273 corr'. y. 100.00 100.00 C10964 S M/Z = 319.9 First peak is baseline drop corrected area. Second peak i s tangent skimmed corrected area. Peak # R. T. min. fi rst sc an max sc an 1a s t peak s c an u i-dt h raw area r 0.000 2 0.000 262 262 0 261 0 261 -1 -1 0 0 Q on d co rr. area 1252 1252 c o rr. * 100.00 100.00 320^32 2 CALCULATION R - G 1o b a 1< 1 ) = . 9835 M/Z = 2 5 7 .0 F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak i s tang en t skimmed c o r r e c te d a r e a . Peak # R. T. min. Fi rst sc an ma x scan 1a st peak scan ui dt h raw area 1 0.000 <ni 0 . 0 0 0 262 262 0 261 0 261 -1 -1 0 0 co rr. area 1557 1557 corr. y. 100.00 10G.00 <320 + 322 )/< 33 2 +334) CALCULATION R -G lo b a l< 3) -- . 0338 < 3 2 8')/< 3 32 + 334 ) CALCULATION R-G 1o b a l( 3 ) = .3981 ^ u^ P J w t a l C\Ci C* C10965 File >G S 171 333 6-334.6 fTiu 2UL UT-3117 SP23 30 200-1/3/25 GT F i l e >GO 171 3 2 1 . 6 - 3 2 2 . 6 a m u . Z U L U T - 3 1 1 7 P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 GT SUR irrr -M C\( C10966 MS data file header from ! >G8171 Sam ple: 2UL UT-3117 O p e r a t o r : GARY MS2 11/09/84 17:37 M i s e : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL#25 BTL#25 Sys. #: 1 MS m o d e l : 87- SU/HW r e v . : CA A L S n : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 Ho. of e x t r a r e c o r d s : 2 Source te m p .: 250 A n a ly z e r tem p .: 265 T r an s f e r l i n e tem p . : 265 Chromat ograph i c tem p eratu res : 200. 250. 0. 0. 0. Chromatographi c tim e s, min. : 1.0 25.0 0 .0 0 .0 0 .0 Chromatographi c ra te , deg/min: 3 .0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t p e ak ii s b a s e l i n e drop c o rre c te d area . S e c o n d p e a k i s t a n g e n t s k i m m e d c o r r e c t e d a r e a . Peak # R. T. min. fi rst scan max s can la s t peak scan width raw area c o rr. area co rr. 1 12.471 259 264 270 11 5 2 6 0 2 35794 100.00 2 12.471 259 264 270 11 52602 30305 84.67 .# M/Z = 3 3 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak i s tangen t skimmed c o r r e c te d a re a . ik R . T . f i r s t max 1a s t peak rni n . scan scan sc an w id th raw area co rr. area corr. y 1 12.4 71 261 264 270 2 12.4 71 261 264 270 9 43S22 9 43322 29237 26222 100.00 89.53 3 3 2 / 3 3 4 C L C U L f i T I OH R - G l o b a K 6> = .8182 M/Z = 3 2 7 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d area. Second peak i s tangen t skimmed c o r r e c t e d a re a . Peak * R. T. min. firs t sc an max scan la s t peak scan width raw area 1 12.491 2 12.491 260 26 265 265 271 271 11 4 0 3 1 6 11 4 0 3 1 6 M/2 = 3 2 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d ar ea . Second peak i s tang en t skimmed c o r r e c t e d a re a . Pe ak # R. T. min. fi rst sc an max scan last scan p e ale wi dt h raw area 1 12.511 2 12.511 263 263 266 266 270 270 7 11639 7 11 6 3 9 co rr. area 25994 22617 co rr. y 100,00 87.01 corr. area 2651 2392 co rr. y. 100.00 90.23 ,_ C10967 S n.'Z = 319.9 First peak is baseline drop corrected area, Second peak is tangent skimmed corrected area. Peak # R. T. min. firs t sc an max sc an 1a s t peak scan width raw area 1 r 12.491 264 265 266 2 4832 2 12.491 264 265 266 2 4832 >Goni co rr. area 1814 1689 corr. 100.00 93. 11 320/322 CALCULATION R - G lo b a K 1) = .6843 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tan g en t skimmed c o r r e c te d a r e a . Peak # R. T. min. f irst sc an max sc an 1as t peak scan width raw area 1 12.531 264 267 26S 4 9999 2 12.531 264 267 268 4 9999 co rr. area 2243 22 : 7 corr. 100.00 9 9 .7 3 <32 + 3 2 2 > / < 3 3 2 + 3 3 4 ) C A L C U L A T I O N R --G l o b a l < 3 ) = .0686 < 3 2 8 *) / <3 3 2 + 3 3 4 ) C A L C U L A T I O N R-Glob&l< 3) = .3990 CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER, rn C10968 Fil* IrU 17 3 F i l >GO 17 3 3 2 1 . 6 - 3 2 2 & amu 2 U L . 2 5 0 3 . ' . 4 3 / . 2 0 3 P 23 3 0 2 0 0 - 1 / 3 / 2 5 0 GT SU BJECT TO PROTECTTVF O P H ers n n r . 6 C10969 MS data, file header from >G0173 Sam ple: 2UL . 2 5 0 3 / . 4 S x .2 0 O p e r a t o r : GARY MS2 11x 0 9 x 8 4 - 1 7 : S8~ M i s e : S P 2 3 3 0 2 0 0 - 1 x 3 x 2 5 0 GT BTL#29BTL#29 S y s . #: 1 MS mode 1 : 8 7 SW/HU r e v . : Cft A L S # : 0 Method f i l e : SP2330 T u n i n g f i l e : AP E 101 No. o f e x t r a r e c o r d s : 2 Source tem p.: 250 A n a ly z e r te m p .: 265 T ra n s f e r 1 ine t emp. : 265 Chromatographi c tem peratures : 200. 250. 0. 0. 0. `p Chromat ograph i c t im e s , m in. : 1 .0 25.0 0. 0 0 .0 0 .0 C h r oma t o g r a p h i c r a t e , d g a r n i n : 3 . 0 0 . 0 0 . 0 0 . 0 0 . 0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s tangen t skimmed c o r r e c t e d a r e a . Peak # R .T . rni n . fi rst sc an max sc an 1a s t peak sc an w id t h raw area co rr. area c o rr, * 1 1 0 .9 3 6 178 188 205 27 95808 59655 100.00 2 1 0 .9 3 6 178 188 205 27 95808 58062 97.33 MxZ = 3 3 1 . 9 F ir s t peak i s base lin e drop c o rre c te d a re a . Second peak i s tangent skimmed c o rre c te d a re a . Peak # R .T . min. f i r st scan max s c an 1a st p e ak sc an w id th raw area c or r . area corr. y. 1 1 8 .9 3 6 183 188 200 2 1 0 .9 3 6 183 188 200 17 6 91 8 5 17 6 91 8 5 45606 43073 100.03 94.45 332x334 CALCULATION R-GlobalC 0) = .7645 fl-'Z = 3 2 7 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s tangen t skimmed c o r r e c te d a re a . Peak it R .T. min. f i rst scan max s c an 1a s t peak sc an w id th -raw area 1 1 0 .9 5 6 183 189 203 20 69961 2 1 0 .9 5 6 183 189 23 20 69961 Mxz = 3 2 1 .9 F i r s t peak i s b a s e lin e drop c o rre c te d are a . S e c ond p e a k i s t a n g e n t s k i rnrned c o r r e c t e d a r e a Peak # R .T . min. f i rst scan max s c an 1a s t peak sc an wi dt h raw - ar ea 1 1 0 . 9 5 6 184 189 196 12 3 8 0 0 7 2 1 0 . 9 5 6 184 189 196 12 3 8 0 0 7 f .. SU BJECT TO PROTECTIVE O R P iF O c o rr. area 41921 39711 corr. y. 100.00 94.73 co rr. ar ea 22143 20871 corr. yt 100.00 94.26 G10970 s M Z = 319.9 Fi-rst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak it R. T. min. f i rst sc an max sc an 1a s t scan peak u i-dt h raw area 1 r. 1 0 . 9 5 6 184 139 201 2 1 0 .9 5 6 184 139 201 17 4 0 2 1 4 17 40214 c o rr. area 17842 16966 c o rr. y. 100.00 95.09 320^322 CftLCULftTION R- G1o b a l < 1) = .8058 M-'Z = 2 5 7 . 0 F i r s t p e a k ii s b a s e l i n e drop c o rre c te d a re a , S e c o n d p e a k ii s t a n g e n t s k i m m e d c o r r e c t e d a r e a . P e ak # R T f i r s t mi n . scan max scan la s t scan peak w id th raw area 1 1 0 .9 5 6 185 189 193 2 1 0 ,9 5 6 185 139 193 8 22850 8 22350 c o rr. area 9898 8498 c o rr. y. 100.00 85.86 <3 20 + 3 2 2 >/< 3 3 2 + 3 3 4 ) C f t L C U L f t T I O N R - G 1o b a l < 3) 3799 <32S')/'<332 + 334) CftLCULftTION R-G 1o b a l< 3) = .3904 SU BJECT TO PROTECTIVE ORDER. Cl0971 File >60174 33.6- 354.0 amu.2UL 2.503/. 43/ .20 2 F 2 33 2GO-1/3/2S0.. jST.. F i l e > 6 0 1 7 4 3 2 1 . 6 2 2 . 6 -amu UL 2 . 5 3 / . 4 8 / . 2 0 P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. ^ C10972 MS data file header from : >G0174 Sam ple: 2UL 2 . 5 0 3 / . 4 8 / . 2 9 O p e r a t o r : GfRY MS2 1 1 / 9 9 / 8 4 -1-31 Mise : SP 2330 2 9 9 - 1 / 3 / 2 5 0 GT BTLtt41B T L # 4 1 Sys. t: 1 MS mo d e l : 8 7 SW/HU r e v . : CR R L S tt : 0 Method f i l e : SP2339 Tuning f i l e : fiPEI91 Ho. o f e x t r a r e c o r d s : 2 Source te m p .: 250 fin a ly ze r te m p .: 265 T r a n s f e r 1 i ne temp.. : 265 . Chromatographi c t em peratures : 299. 250. 0. 0. 0. Chrom atographic t i mes, min. : 1.9 2 5 .0 0 .0 0 .0 0 .0 Chromat ographi c r a t e , deg/m in: 3 .0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s tangen t skimmed c o rre c te d a re a . Peak tt R. T. min. fi rst scan max scan 1a s i peak sc an w id th raw area co rr. area c o rr. ym 1 12.552 260 268 278 18 98047 76015 100.00 12.552 260 268 278 18 98947 71083 93.51 M/Z = 3 3 1 . 9 F i r s t peak i s b a s e 1i ne d ro p c o r r e c t ed a r e a . Sec ond peak i s tangent skimmed c o rre c te d a re a . Peak tt R. T. mi n . fi rst sc an max scan 1a s t pe ak sc an w id th raw area c o rr. area corr. * 1 12.552 269 268 285 25 92933 61233 100.00 2 12.552 260 268 235 25 92933 59658 9 7 .4 3 332/334 CALCULATION R - G 1o b a l (. 0> = . 8055 M/Z = 3 2 7 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s t angent skimmed c o rre c te d a r e a . Peak # R .T . min. f i rst sc an max scan 1a s t scan peak w id th raw area 1 12.572 262 269 282 20 81762 2 1 2 .5 7 2 262 269 282 29 81762 M/Z = 3 2 1 . 9 F i r s t peak i s b a s e lin e drop c o rre cte d a re a . Second peak i s t angent skimmed c o r r e c te d a r e a . Peak tt R .T . min. f i rst sc an max scan la s t peak sc an w id th raw area 1 12.572 259 269 2 12.572 259 269 CONFIDENTIAL SUBJECT TO DPOTCY-rnnr /vonro 289 289 30 334113 30 334113 corr. area 57192 54482 corr. y. 100.00 95.41 co rr. area 298113 287268 c o rr. y. 100.00 96.36 C10973 s M/Z = 3 1 9 . 9 Fi r s t peak is b a s e lin e drop cot' r e e l e d a r e a . Second peak i s t angent skimmed c o rre c te d a re a . Peak # R .T. min. firs t sc an rna x c an 1as t peak s c an w i-dt h r au area 1 ,, 12.572 253 269 284 2 12.572 258 269 284 26 248367 26 248367 > Q r \l^ co rr. area 217141 206078 c o rr. * 100.00 94.91 320/322 CALCULATION R - G 1o b a l < 1 ) = .7284 M/Z = 2 5 7 . 0 F i r s t pe ak i s b a s e 1 i ne d ro p c o r r e c t e d a r e a . Sec ond peak i s t a rg e n t skimmed c o r r e c t e d a r e a . Peak tt R .T. mi n . f i rst scan max scan 1a s t scan peak w id th raw area 1 12.572 259 269 285 2 12.572 259 269 . 285 26 156236 26 156236 co rr. area 119342 114285 corr. Ji 100.00 9 5 .7 6 <320 + 3 2 2 )/< 332 +334) CALCULATION R-Gl obal < 3) = 3 .7 5 4 2 < 3 2 8 ')/< 3 3 2 + 334) CALCULATION R - G 1o b a l ( 3 ) = .3965 SUBJECT TO PROTECTIVE O R D ER C10974 P i l e * >G17 5 3 3 3 . 6 - J -.i 4 . 6 arti u . 5IJL 2 5 . 0 3 / . 4 3 / . 2 0 SP2330 200-1^-3/250 ...CT ... F i l e >GO 1 7 5 3 2 1 . 6 - 3 2 2 . 6 a m u . S U L 2 5 . 0 3 / . 4 3 / . 2 0 P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 . . . GT-. CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. . C10975 MS data file header from : >G0175 Sam ple: 2UL 2 5 . 0 3 / . 4 8 / . 2 0 O p e r a t o r : GARY MS2 1 1 / 0 9 / 8 4 * 9 : 3 9 ---- Mise : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL#43BTUt43 S y s . ft: 1 MS m o d e l : 8 7 S U / H U r e v . : Cfl A L S ft : 0 Method f i l e : SP2330 Tuning f i l e r RPEI01 No. o f e x t r a r e c o r d s .: 2 Source tem p,: 250 A n a ly z e r tem p .: 265 T r a n s fe r lin e temp. : 265*--'- ? Chromat ograph i c t emperat u r es : 200. 250. 0. 0. 0. Chromat ograph i c tim e s , min. : 1 .0 25.0 0 .0 0 .0 0. 0 C h r o m a t o g r a p h i c r a t e , d e g / mi n : 3 . 0 0 . 0 0 . 0 0 . 0 0 . 0 M/Z = 3 3 3 . 9 F r s t peak i s b ase 1 i ne drop c o rre c te d a re a . S e c o n d p e a k i s t a n g e n t s k i mmed c o r r e c t e d a r e a . Peak it R.T. f ir s t mi n , sc an max scan 1a s t peak scan width raw area co rr. area corr. y. 1 1 2 .7 5 4 272 278 281 2 1 2 .7 5 4 272 278 281 9 53015 46495 100.00 9 58015 38048 81.83 M/Z = 3 3 1 . 9 F i r s t e ak i s b a s e l i n e drop c o rre c te d a re a . Sec ond peak i s t a n g e n t skimmed c o r r e c t e d a r e a . Peak it R.T. ,fi rst min. sc an max sc an 1as t pe ak sc an w id th raw an e a co rr. area corr. y 1 1 2 .7 5 4 272 278 281 2 1 2 .7 5 4 272 278 281 9 48399 37333 100.00 9 43399 30-611 80.80 332/334 CALCULATION R-GlobalC 0) = .8148 M/Z = 3 2 7 . 9 F i r s t peak i s b ase 1 i ne drop c o rre c te d a re a . Second peak i s tangent skimmed c o r r e c te d a r e a . Peak ' ft R .T . min. firs t scan max scan 1as t peak sc an w id t h raw area 1 12.774 273 279 282 2 12.774 273 279 282 9 53142 9 58142 M/Z = 3 2 1 . 9 F i r s t peak i s base 1i ne cirop c o r r e c t e d a r e a . Secon d p e ak i s t a n g e n t skimmed c o r r e c t e d a r e a . Peak ft R .T . min. firs t sc an max s c an 1a s t peak sc an w id t h raw area 1 12.774 269 279 282 2 12.774 269 279 232 CONFIDENTIAL 13 1 7 3 6 7 5 3 13 1 7 3 6 7 5 3 C larity*^ com . area 46883 39143 com . ar ea 1721712 1282812 co rr. y. 100.00 83.49 c or r . * 100.00 74.51 . C10976 s M/Z = 3 1 9 . 9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R. T. min. fi rst sc an max scan la s t peak sc an wi dt h raw area 1 , 1 2.7 74 270 279 282 2 12.774 270 279 282 12 1267934 12 1267934 c o rr. area 1253342 948926 co rr. A 100.00 75.71 320/322 CALCULATION R-G lobalC 1) = .7280 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak is tangen t skimmed c o r r e c t e d a r e a . Peak 4 R .T . min. f i rst scan max scan 1a s t peak scan width raw area 1 12.774 276 279 282 2 12.774 270 279 282 12 7 0 7 0 1 5 12 7 07 0 1 5 co rr. area 691091 517709 c o rr. >: 100.00 74.91 C3 2 0 + 3 2 2 ) / <3 3 2 + 3 3 4 ) C A L C U L A T I O N R-Global< 3) = 3 5 .2 5 8 b < 3 2 8 ')/<332 + 334) CALCULATION R -G lo b al< 3) = .3720 SUBJECT TO PROTECTIVE ORDER, nnrxyy^ C10977 vino i e : 2 U L 1 0 0 2 / .'>8 / . 2 9 O a e r a t o r ! KOY ni -c bP2339 20 0~1 / 3 / 2 5 0 B 1 L * 0 3 BT l I `.3'}S . 1 l Mb M o d e l : 37 Sk l / H W r e u . : CA M erli od f i l e ; 8 P 2 3 3 G 1un i n a f i i e = A P t l O i '5 o u r c e t e n p . i 2 5 0 A n a ly z e r tenp.= 0 nb L 1 / 9 5 / :J4 A L 8 fr 0 N o . o+ e x i r a r e c o r a s T ra n s fe r Line te n o . 0 n C hro nato g rap hic C hro nato g rap hic Chr o nato g rap h ic te n p e ra tu re s t in e s, n in . r a t e , deq /n in = 0. 0.0 0.0 . 0.0 0.0 0. 0.0 0.0 0. 0.0 0 . [j 0 0 .0 0 .9 i \' : : -= y * * . ? f )r s t p e a k i s b a s e l i n e drop c o rre c te d a re a . Second peak is Tangent sk in n e d c o rre c te d a re a , Peak =r K.1. first nin . scan na x la st scan . scan peak w id th raw area corr . area c or r . i "Vi 1 2 .3 3 5 12 .335 24? 24? 255 255 267 267 is 42807? 18 4 28 9 7? !'1 ' L " 3 3 :i. . 9 r 1 rs t pea k i s b a s e lin e drop c o rre c te d area . Second peak is tang en t skin n e d c o rre c te d a re a . 581Si ^ 375528 i 0U. 00 9 8.4 3 l:; e a k .% k . r . firs t nin . scan na x scan la st scan peak w id th raw area corr . area corr . /k i i 2 .3 3 5 24? i 2 .535 . 24? 255 255 266 266 i7 359343 30884* 1 U0 . 00 17 350343 3 0i ? 8b 9 7 .7 8 .j 5 2 / ,.)34 C A L C U L A T 1 0 N ft-Globa1C 0 ) = .8095 ri ~ 52/ .? i-ir*st peak is baseline drop corrected area . Second peak is tangent skinned corrected a r e a , Peak :ir k .T . firs t nin . scan nax scan la st scan peak w idth raw area i 1 2.355 1 2 .3 5 5 250 250 256 256 267 267 17 409322 i 7 409322 u-'i - 521 .9 f i r s t peak is b a s e lin e drop c o rre c te d a r e a . Second peak 'is tan g en t sk in n e d c o rre c te d a re a ak K .T . fir s t * n in . scan 1 12.355 2 12.355 251 251 i^ 1 lo 1 U nax scan 256 la st scan 26? peak w id tn 18 raw area 135239 13523? corr . area 366482 3 5 8 2 ii corr 7. i o9 . 00 9 7.7 4 corr. area 88 043 87584 corr . / ii 1 U 0 . 0 (J 99.1 8 C10978 n _ - j i / . V F i r s t peak i s b a s e lin e drop co rre c te d are a, second peak i s tangent skinned co rre c te d a re a , Peak * k,.T. f i r s t nin . scan nax scan la s t peak scan width raw area 1 1 2.355 250 256 267 2 12.355 250 256 267 17 117120 i 7 i 17 i 2b ' c orr . area 71755 69733 \ corr . V 100.00 97.25 320/322 CALCULATION R-GlobaU i) = .81S 0 h * t ~ 2 S'/ . ') F i r c t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s tangent skinned c o rre c te d a re a . Peak * K .T . f ir s t nin . scan na x scan la s t peak scan width raw area 1 12.355 2 12.355 252 252 256 256 264 264 12 85928 12 85928 c or r . area 424 04 38954 corr . / i 00 . 00 91.86 20 + 3 2 2 ) / \ 3 3 2 '+*3 3 4 ) CA LC UL A TI O N R-GiobaiC 3 ) = .2315 <3 2 b '* >/ ( 3 3 2 + 3 3 4 > CA LC UL A TIO N R-Global* 3 ) = .5297 CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. C10979 Fils >3114 333.6-334.6 imu.^UL UT 3041 S P 2 3 3 0 2 0 0 -1 ^ 3 /2 5 0 GT BT F ile - >E 3 1 1 4 3 2 1 . 6 - 3 2 2 . 6 am u .S U L U T -3 0 4 1 S P 2 3 3 2 0 - 1 / 3 / 2 5 0 GT BT CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER nnrkyyty G10980 g : t i i l i e n a a r f r' o n B i l i 4 C a m o l e - 2 U L UT - 3 0 4 1 O p e r a t o r : HQY GTi r i s e = 5 P 2 3 3 Q 2 0 0 - 1 / 3 / 2 5 0 BTLI3 BTL.+ 31 nb i i / 0 5/ : h* 1. ; 0 0 Svs . : 1 rib m o d e l : 8 7 SUl/HW r e v . CA Method - file = SP2330 ' T u n i n g f i 1 e : AP I i So u r e e t e m p . : 250 A n a l y z e r temp 0 ALS # 0 No. of e x t r a r c o r d s : Tr a ns f e r 1 1ne temp. 2 0 Chrom atographic Chj~ orna t o g r a p h i c Chrom atographic tenperatores t m e s , min . : r a t e , deg/min = 0. 0.0 0 . 01 0. 0 .0 0.0 0. 0. 0 .0 0 0.0 0.0 0. 0.0 0.0 li ' 1 - 3 3 3 . 9 r i. r s t p e a k i s b a s e l i n e crop co rre cte d area . Second peak is : tangent s k m n e o c o r r e c te d a r ea . Pea k * ii . T . n in . fir s t scan max scan la s t scan peak wi dt h raw area corr . area corr . X i 12.354 2 i 2 .354 25 0 250 256 256 268 268 IS 242036 18 2 4 2 0 3 6 M *'7. - 3 3 1 . 9 F i. r s t p e a k i s b a s e l i n e d r op c o r r e c t ed a r e a . Second peak isi ta n g e n t skimmed c o r r e c t e d a re a . 197666 i V 2950 1 0 0 . 0 vi 9 7 . 61 Peak * P . . f i rs t min . sea n max scan la s t scan peak w id th raw area c or r . area corr. V i 12.354 3 1 . 3 5 4 25 0 250 256 256 266 266 16 2 0 0 0 8 0 i6 - 200080 160080 156912 100 00 9 3 . 02 3 3 2 / .5*34 C A L C U L A T I O N P - G 1 ob a 1 ( 0 ) = .8099 T 327.9 su b jec t' F i r " t p o a K 3. s b a s e l i n e drop c o rre c te d are a . Second peak is tangen t skimmed c o rre c te d a re a . Pea k i ;a K .T . min . 12.375 12.375 fir s t scan 251 25 i max scan 257 257 la s t scan peak w id th 268 268 17 17 raw area 233202 233202 ti Z - 3 2 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak is tangent skinned c o rre c te d a re a . Peak # K .T . fir s t min . scan ma x scan la s t scan peak w id th raw area 1 12.375 254 257 264 10 3 6 0 4 3 2 12.375 254 257 264 10 36 043 1 OTECTVE ORDER, ; . . * c or r . area 188373 133859 corr . " i 00 . 00 97.60 C10981 corr . area 10543 9 3 i3 corr. / U0.U t w 88.33 -'S n / - 319.9 Fir-: i pi?ak is baseline drop corrected area. Second peak is tangent skinned corrected area. ia k K . T . f i r s t na x la s t peak * nin . scan scan scan width raw area i 12.375 253 257 264 ii 3714? 2 12.375 253 257 264 ii 37149 y j/-2J '*<** , , corr . area 9308 8466 c or r . /u i u o . ou 9 0.95 320/322 CALCULATION R-GIobali i) - .8 8 2 9 n/Z - 257.0 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak is tangent skin n ed c o rre c te d a r e a . Pea k HF R. I . first nin . scan na x scan la s t scan peak w id th raw area 1 12.375 2 12.375 252 252 257 257 260 260 8 35813 8 35813 corr. area 6421 6121 corr . X 100.00 9 5 .3 3 520 + 3 2 2 ) / < 3 3 2 + 5 3 4 ) C A L C U L A T I O N R-GiobalC 3) = .0555 <328- >/<332 + 534 ) CALCULATION R -G lo n a li 3) - .5263 SU BJECT TO PROTECTIVE O R D ER C10982 F i l e '>B 3 1 15 J ; D-334.6 StfliU 2 UL U T - 3 0 4 2 3 P2330 2 0 0 - l - ' 3 / 2 5 0 GT" ~ BT F i l e >3115 3 2 1 .6 - 3 2 2 .6 amu.SUL UT-342 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BT 4600- 010.0 10.5 ______ 'I 1 1 1 1 I ' ' 1 I ' 1 1 1 I 1 1 1 1 I 11.0 11.5 12.0 12.5 13.0 co nfidential SUBJECT TO PROTECTIVE ORDER, n n 8 o i ^ 1r 13.5 14.0 14.5 15.0 C10983 n V? `.i a t 3 t i l e h e a d e r i r o n >B 3 1 1 S F a n n i e : 2 UL U T -3 0 4 2 O p e r a t o r : ROY MS ii/O S/84 i = hi s r = S P 2 3 3 0 2 0 Q - 1 / 3 / 2 5 0 GT BTL433 BTL433 b v 3 . 1= i MS m o d e l : 8 7 S U / H W r e v . : C A A L S 4 = 0 Method f i l e : SP2330 T u n i n g f i l e : A P E I 01 No. of e x t r a r e c o r d s 2 S o u r c e t e m p .= 2 5 0 A nalyzer temp. : 0 T r a n s f e r .1 i n s t e m p . 0 Chrom atographic C l \ r orna t o g r a p h i c C h r orna t o a r a p h i c tem peratures t imes , m in . rate* deg/m in: 0. 0.0 0.0 0. . 0.0 0. 0. 0.0 0. . 0. 0. 0 . t) 0.0 H/ l - 3 3 3 .? F i r s t pea is b a s e lin e drop c o rre c te d a re a . Second peak i s Tangent skimmed c o r r e c t e d a r e a . Peak . * R .T. min . fir s t scan i 12.354 [`J 1 2 . 3 5 4 250 250 max l a s t scan scan 256 256 26a 266 peak w id th 16 16 raw area 15441 154401 c orr . area 115793 i 13657 corr . "/ 100 . 00 98.. 16 h / I - `3 3 i . 9 F i r s T peak i s b a s e lin e d r op c o r r e c t e d a r e a . S e c ond pea k i s t a n g e n t skim m ed c o r r e c t e d a r e a . Peak 4 R .T . f i r st min . scan ma x scan la s t scan peak w id th raw area c or r . area corr . X i 12.354 2 12.354 250 250 25 25a 265 265 15 1 2 8 6 78 15 i 28678 91898 9 04 i 3 1 00 . 00 98.38 j 32 / 3 3 4 CAL CUL AT 1 0 N R- G lo b a li 0) = .7930 ri/K - 3 2 7 .9 F i r s t peak is b a s e lin e SUBJECT r e PROTECT.''/: drop c o rre c te d area . ORDER. Second peak i s tangent skimmed c o r r e c t e d a re a . Peak 4 k .t . min . Firs t scan ma x scan la s t scan peak w id th raw N area f corr . ar ea corr' . /. 1 12.375 *3 1 2 . 3 7 5 ri/Z ~ 3 2 i . 9 252 252 257 257 265 265 13 147687 13 i 4 7 8 8 7 113554 109824 l 0 0 . Q0 96.48 F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak is t angen t skimmed c o rre c te d a re a C10984 Pea k 4 ft. T . f i r s t min . scan 1 12.375 2 12.375 253 253 ma x scan 2 57 257 la s t scan peak w id th 262 262 9 9 raw area 367975 367975 corr . ar ea 331687 313439 corr". /I i\{ 100.00 9 4 ..50 ri / ~ 3 i 9 . 9 .. F 1. r s t p e a k i s b a s e l i n e drop c o rre c te d area . S e c o n tj p e a k i s t a n g e n t s k i M M e d c o r r e c t e d a r e a . Peak i K .T . firs t run . scan nax scan la s t scan pea k w id th raw area i wH p j i i 12.375 12.375 253 253 257 257 262 262 9 3 05 2 i 5 9 305215 ^ 33 r 5 corr . area 271699 257758 corr , X 1 0 0 . 94.87 ^20/3 22 CALCULATION R - G lo b a 1( 1) = .8191 ri/2 = 257.0 F i. r s t p e a k i s b a s e l m e drop c o rre c te d area . Second peak i s tangent skin n e d c o rre c te d a re a . Peak t R .T. f i r s t nin . scan Max scan la s t scan pea k w id th raw area i 12.375 "J 1 2 . 3 7 5 254 254 257 257 262 262 8 195226 3 195226 n o f -J area 157882 150626 cor r . X 10 0 . 00 95.40 (320 + 322>/<332 +334) CALCULATION R -C lo b aK 3) = 2 .9 0 5 2 k3 2 8 -')/(3 3 2 + 334) CALCULATION R - G l o b a l ( 3 ) = .5324 L i i n r 4 :V > c i'.C > n rT SU B JEC T TO PROTECTIVE C R D B L ' v^ C10985 F i l e >E3116 3 3 3 . - 334 a mu 2 U L U T - ' 3 0 4 3 SP2330 200-1^3^250 5T BT ' S G0 0 0- 40000" J \ ________ A . A 0 10.0 10.5 11.0 11.5 12.0 L | -JI \I _T__j___.__1_-_T_j__1_______| _'__I _____| _-._____I_ 1 2 .5 13.0 13.5 14.0 14.5 15.0 F i l e >B 3 1 16 3 2 1 . 6 - 3 2 . 6 amu IJL U T - 3 0 4 3 SP 23 30 2 0 0 - 1 ^ 3 ^ 2 5 0 GT BT 100000" 50000-- > r~> < 10.0 10.5 11.0 |~1 1-1 1 '~T l " 11.5 12.0 U. 12.5 13.0 oooci SUBJECT TO PP.OTECnVE ORDER. 13.5 14.0 14.5 T s .o C10986 First peak is baseline drop corrected area. Second peak is tangent skinned corrected area. Peak * R.T . firs t nin . scan na x scan la s t scan peak w id th raw area i 12.375 2 i 2.375 254 254 257 257 262 262 B 646715 8 646915 c or r . area 598907 575623 cor." . X 100.00 9 6 .il \p n / 'z v ^ C A L C U L A T I O N R - G I o b a 1 ( 1 ) =' .8303 ri / L ~ 2 5 7 . 0 F :i.rst peak i s b a s e l i n e drop c o rre c te d area . S e c o n d p e a k 1 si t a n g e n t s k i n n e d c o r r e c t e d a r e a . Peak * R . T. f i r s t nin . scan nax scan la s t scan peak w id th raw area i^ t i 2 .3 7 5 2 12.375 254 254 257 257 262 262 8 374852 Q 374852 c orr . area 313020 311824 corr . /m too. 0 98.05 <320 + 3 2 2 )/ '< 3 3 2 + 3 3 4 ) CALC U LA TIO N R - G l o b a l <' 3 ) = 4 .327i <32 B ' ) / ( 3 3 2 + 3 3 4 ) CALCULATION R ~ G 1 ci b a I < 3 ) = .5085 t , L ' | _[ ^SU B JEC T TO PROTECTIVE ORDER- n O 'JS S C10988 File > B31 17* 333.6-334.6 amu.2 UL UT-3044 SP233 200-1 '3/250 GT BT F i l e >B3 117 321 . 6 - 3 2 2 . 6 -mu.SUL U T -3 0 4 4 S P 2 3 3 0 0 0 - 1 / 3 ^ 2 5 0 GT BT if ' A T SUBJECT TO PROTECTIVE ORDER. i? C S K C10989 ri 5 a $ T a f i 1 e h e a d e r f r o >B 3 i 1 7 b a n n i e : 2)IL u r - 3 0 4 4 O p e r a t o r ; IVQY Mi s c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL*37 BTL*37 MS i 1/05/84 9vs . * ! i MS n o d e ! : 8 7 SW/ HW r e y . C A A L S 0 Method filer S P 2 3 3 0 Tuning f i l e r APEI01 No. o f e x t r a r e c o r d e -Sour ce t e n p . - 2 5 0 Analyzer tenp.; 0 T ra n s fe r lin e tenp . 2 :0 0 0 C h ro n a to g ra p h ic Ch/` ona to g r a p h i c C h ro n a to g ra p h ic tenperatures : tin e s, n in . ra te , deg/nin; . 0.0 0.0 0. ` 0.0 0.0 0. 0.0 0.0 0. 0 .0 0.0 0. 0.0 0 .0 h/Z - 3 33 .9 F i r s t peak is b a s e lin e drop c o rre c te d area. Second peak is tangent skinned c o rre c te d a re a . Pea k t R .T . f ir s t nin . scan nax la s t scan scan peak w id th raw area corr . area corr . X 1 12.355 2 12.355 250 250 256 256 266 266 16 2 2 9 6 6 8 i 6 229668 190628 185956 10 0 . 0 0 9/ . 55 M/Z - 331.. 9 First- peak l s b a s e lin e droo c o rre c te d area . Second peak i s tangent skinned c o rre c te d a re a . P ea k # K .T . f ir s t nin . scan nax scan la s t scan peak wi d t h raw area c or r . area c or r . /h i 12.355 c_ 1 2 . 3 5 5 250 250 256 256 264 264 i4 191754 155214 100.00 i 4 191754 150629 9 7.0 5 3 3 2 / 3 3 4 CALC UL A T I ON R - G lo b a 1( 0) - .8142 F i r s t peak is b a s e lin e drop c o rre c te d Second peak is tangent skinned c o rre c te d Peak * R .T . firs t nin . scan nax scan la s t peak sc a n 1 width raw area i 12.375 2 12.375 251 251 257 257 ' 265 265' 14 2 2 6 6 3 9 14 2 2 6 6 39 ri / Z - 3 2 1 . 9 r *i r s t p e a k i s b a s e l i n e drop c o rre c te d area. S e c onci1 p e a k i s t a n g e n t s k i n n e d c o r r e c t e d a r e a . Peak % -- 1 2 IV . T . nin . -- 12.375 12.375 firs t scan -- 254 254 nax scan _________ _ 257 257 la s t scan _____ 262 262 peak w id th _ _ _____ . 8 8 raw area ________ _ _ _ __ 154102 154102 c orr . area 179165 i 72774 corr . X 100 . 00 9 6 .4 3 C10990 c orr . area 120374 i 17538 corrv X /W i 00 . 00 97.64 S rl /' > = 's i ? . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak is tangent skinned c o rre c te d a r e a . -1 Peak * fir s t nin . scan na x scan la s t scan peak w id th raw area i 12.375 12.375 * 254 254 257 257 262 262 8 130072 8 130072 O 15 - 1 ' corr . area 97976 96132 corr . % i ao. o 9 8 .1 2 320/322 CALCULATION R-GlobaiC i) - .8139 ft/7. 257.0 F i r s t peak is b a s e lin e d r op c o r r e c t e d a r e a . Second pea k i s tangent sk in n e d c o r r e c t e d a re a . Peak # ft . T . f i r s t nin . scan 1 12.375 2 12.375 254 254 na x scan 257 257 la s t scan 263 263 peak w id th o 9 raw area 101154 101154 corr . area 55704 54903 corr. 7. 100.00 9 8 .5 6 -:30 + 3 2 2 ) / < 3 3 2 + 3 3 4 ) C A LC U LA T IO N ft- G l o b a l i 3 ) = .6314 328' >/< + 334) CALCULATION R- G lo b a li 3) - .3149 , \SUBJECT TO PROTECTIVE ORDER. C10991 F i l e >E 3113 4 . * mu.^UL UT 0 4 5 1 P 2 3 3 0 2 O 0 - 1 / 3 / 2 5 0 GT BT F i l e >33113 3 2 1 .6-3 2 2 itiu . 2UL U T - 3 0 4 5 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BT j SUBJECT TO PROTECTIVE ORDER. o n r* p q G10992 nS '1a T a il le n e a d e r t'rnn : >B3i i8 ^aMDlS! 2 U L U T - 3 U 4 5 O p e r a t o r : ROY MS 11/03/04 2 h i s c ; SP2330 2 0 0 - 1 / 3 / 2 5 0 CT BTL=U=39 B T L * 3 9 Svs. t i MS M od el 5 8 7 S W / H U r e v . : CA A L S t : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 No. of e x t r a r e c o r d s 2 S o u r c e t e n p .= 25 A n a ly z e r tenp . Transfer lin e tenp. t) C h ro n a to g ra p h ic Ch." ona t o g r a p h i c C h ro n a to g ra p h ic tenperatures : tin e s} n in . = r a t e , deg/nin = 0. 0.0 0.0 ' Q. 0.0 0.0 0. 0.0 0 .0 0. 0 .0 0.0 0. 0 . o.0 rf/Z - 3 3 3 .9 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak i s tangent skinned c o rre c te d a re a . Peak * K .1. f i r s t nin . scan na x scan la s t scan peak w id th raw area i 12.355 2 12.355 251 251 256 256 267 267 16 1 9 5 0 19 16 195019 corr . area 153195 150411 corr . 5C 10 0 . 00 9 8 .1 8 ri/Z - 3 3 1 .9 F i r s t p e a k :i s b a s e l i n e d r op c o r r e c t e d a r e a . S e c ond p e a k i s t a n g e n t s k i n n e d c o r r e c t e d a r e a . Peak T k .T . fir s t nm . scan na x scan la s t scan peak w id th raw area 1 12.355 2 12.355 252 252 256. 256 267 267 15 162092 15 1 6 2 0 92 c or r . area 126212 123227 corr. " 100.00 9 7 .6 3 3 3 2 / 3 3 4 CALCULAI ION R - G l o b a l ( 0) = .8239 -v - p / F i r s t peak i s b a s e lin e drop Second peak is tangent skinned corrected corrected .3*** -~ i - -- i area. area. ij -- uJA :n O r r C 7 ! V E O R D ER . Peak * R .T. f i r s t nin . s can na x scan la s t scan peak w id th raw area c or r . area corr . X 1 12.375 2 12.375 251 251 257 257 265 265 14 187228 147034 10 0 . U0 14 187223 143632 97.69 H/Z ~ 3 21 .9 F i r s t p e a k :l s b a s e l i n e drop c o rre c te d area . Second peak i s tangent skin n e d c o rre c te d a r e a . Peak * R .T . firs t nin . scan na x scan la s t scan peak w id th raw area 1 12.375 n 12.375 254 254 257 257 262 262 8 1686B7 8 168687 C1Q993 corr. area c orr . X 143415 135535 100.00 94.51 n / i 1 9 .. 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak is tangent sk in n e d c o rre c te d a re a . Pea k t R .T . fir s t nin . scan na x scan la s t scan peak w id th raw area 1 12.375 O&_ 1 2 . 3 7 5 254 254 257 257 262 262 8 140123 3 140123 y. a z< , ' / O j II - c Qr r . area 114939 109047 c or r . /. 10 0 . 0 9 4 .8 7 `5 2 0 . / 3 2 2 C A L C U L A T I O N R - G l o b a K i) = .8014 n *Z 2 5 7 . 0 F i r st peak is b a s e lin e drop c o rre c te d area. Second peak is tangent skin n ed c o rre c te d a rea . Peak 4 R . T. f i r s t nin . scan na x scan la s t scan peak w id th raw area 1 12.375 fOc- 1 2 . 3 7 5 254 254 257 257 262 262 8 98062 8 93062 corr . area 64206 62230 corn . X i 00.00 9 6 .9 2 <320 + 3 2 2 ) / < 3 3 2 + 3 3 4 ) C A L C U L A T IO N R - O l ob a 1 C 3 ) - .9247 '!328` >/<332 + 334) CALCULATION R - C l o b a l C 3 ) = .5216 SUBJECT TO PROTECTIVE ORDER. C10994 S) ~ Tl t " g 3i 'J J ) H ro li G* V n M- Itli M >! c> V W i.0 w 10 :o ro ro B C ro ro \ 4^ C roo t-> TJ ro c ro o \ CO ro tn w *-* cn S1 G> Q Ci o ili _ 01 Ol IO ro 01 co. Co Ol -T- Ol 1 cn_ w ^ *"* co ro -j o. Ol i V i ro co o. il' 3 C ro c cn u> X1 i 1 1 1 i- 1 1 ro 'Si ro * C ro oi1 ro to_ <-) TJ ro -- co co co cn ro i *-* \ co \ IO cn v W oi_ w W Cj cn o LO co co a. Co Co -ro> v3C< IO L_ r~ ro \ -u co D IO \ lo Ol l i d a t a file header fron >B 3 i i 9 a mp 1. b ; 2 U L 1 . 0 2 / . 4 8 / . 2 0 Hi sc P2330 2 0 0 -1 /3 /2 5 0 O p e r a t o r ; ROY B T L *0 S BTL& 5ys . +! i HS r i o d e l ; Method file - - SP233Q 8 7 SW/HU r e v , : CA Tuning f i l e ; APEIOi * S o u rce t e n p .; 250 Analyzer ten p .; 0 HS 5 i1 / 0 5 / S 4 ALS * : 0 No. o f e x t r a r e c o r d s - Transfer lin e tenp. 2-43 2 0 Chronatographic Ch-r ona t o g r a p h i c Chronatographic tenperatures tin e s , nin . r a te , deg/nin 0. 0.0 - 0.0 0. 0.0 0.0 0. 0.0 0 .0 0. 0 .0 0.0 0. 0.0 Q. 0 M/Z = 3 3 3 .9 F i r s t peak i s b a s e lin e d r op c o r r e c t e d a r e a , Second! peak i s tangent sk in n e d c o r r e c te d a re a . Peak * R .T . f ir s t nin . scan nax ' la s t scan scan peak w id th raw area corr . area corr . 7. 1 12.334 2 i 2.334 25 i 25 i 255 255 264 264 13 420210 389543 i 00 . 00 13 420210 3 81 2 42 9 7 .8 7 ri/Z - 33 i . 9 F i r s t peak is b a s e lin e drop c o rre c te d area . S e c o n d p e ak i s t a n g e n t s k i n n e d c o r n e c t ed a r e a . Peak * k .T . f i r s t nin . scan na x scan la s t scan peak w id th raw area corr . area .corr . X i 12.334 2 2.334 250 250 255 255 265 265 15 355362 317997 100.00 15 355362 3 1 1 6 6 7 9 8 .0 1 3 3 2 / 3 3 4 C A L C U L A f XON R -G lobaK 0 > = .8163 ri/Z = 3 2 7 .9 F i r s t peak is b a s e lin e drop c o rre c te d Second peak is tangent skin n ed c o rre c te d Peak * R .T . first n in . scan i 12.355 2 12.355 252 252 nax scan 256 256 la s t scan 266 266 peak width 14 14 raw area 424 061 424 0 i rt/Z - 3 2 1 .9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak is tangent skinned c o rre c te d a r e a . Peak * k .T . firs t nin . scan i 12.375 'D 1 2 . 3 7 5 252 252 nax scan 257 257 la s t scan 266 266 peak w id th 14 14 raw area 77486i 774861 corr. area 388935 380493 corr . / 10 0 .,0 0 97,83 C10996 corr . area 739973 726127 corr . r* i 0. 00 98.13 H/Z =319.9 F i r s t peek is b a s e lin e drop c o rre c te d are a . Second peak i s tangent skinned c o rre c te d a r e a . R . I . firs t nin . scan nax scan la s t scan peak w id th raw area 12.375 12.. 3 7 5 25 0 250 257 257 266 266 16 644133 16 6 44133 __ -. ' & .i . T 'I corr . area 60238? 587541 corr . 7. i 00 . 00 97.54 320/322 CALCULATION fl- G lo b a 1( 1) = .8 i4 i H/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s tangent skinned c o rre c te d a re a . Peak # k .T. f i r s t nin . scan na x scan la s t scan peak w id th raw area i i 2.375 2 i 2.375 25 i 25i 257 257 265 265 14 3 6 9 0 6 1 i4 36 9 06 i corr . area 321167 311374 corr . X i 00 . 00 9 6 .9 5 <320 + 3 2 2 ) / <332 + 3 3 4 ) C A LC U LA TIO N R - G l o b a 1< 3 ) = i . 8972 <3 2 S / ) / ( 3 3 2 + 3 3 4 ) C A L C U L A T I O N R - G l ob a 1< 3 ) = .5403 n r. r. O S U B JtC T TO PROTEO VE ORDER. C10997 File >B31 0 333.6-334.6 amu.ZUL UT-3046 STAB.SP2330 183-1^7/275 3 F i l e >33129 3 2 1 .6 - 3 2 2 .6 amu.2UL UT-3346 TAB.-SP2330 130-1/7/275 B SUBJECT TO PROTECTIVE ORDER, C10998 ,1 3 ile h e a d e r f r o n : > 8 3 1 2 0 ip- 2UL U T-3046 O p e r a t o r : ROY MS 1 1 / 0 5 / 8 4 3 ; OS : B1AB.P233 18 -1/7/275 B T L *5 1 B T L *5 i t i MS n o d e ! : 8 7 S W/ HW r e o . : CA A L S * = 0 thod f i l e : SP2330 Tuning f i l e : APEI01 No . o f e x t r a r e c o r o S : 2 'ce t e n p .: 250 Analyser te n p . 0 Transfer lin e tenp. : U Chrona tog rap h ic te n p e ra tu re s C tiro nato g rap h ic t i n e s , Min. Chrona t ographic r a t e , d e g /n in : 0. 0.a 0.0 0. 0. 0.0 0. 0.0 0.0 0. 0.0 0 .0 0. 0 .0 0.0 = 333.9 st peak i s b a s e l i n e drop c o rre c te d a re a , nd p e a k i s t a n g e n t s K i n n e d c o r r e c t e d a r e a . K .1 . f i r s t nin . scan .2.376 2 .3 7 6 252 252 nax * la s t scan scan peak width. 257 257 266 266 14 14 raw area 214374 214374 corr . area 177596 172948 corr . X 1 0 0 . 00 9 7 .3 8 - 331.9 st peak is b a s e lin e drop c o rre c te d are a , jnd p eak i s t a n g e n t s k i n n e d c o r r e c t e d a r e a . H. T . f i r s t nin . scan na x scan la s t peak s c an width raw area corr . area c orr . X 12.376 12.576 252 252 257 .257 264 264 12 175550 143702 100.00 12 175550 139508 9 7 . 0 8 - 0 4 334 CALCULATION l o b a l( 0) = .8092 ~ 327.9 ' s t peai< i s b a s e l i n e drop ond p e a k i s t a n g e n t s k i n n e d corrected corrected *\ t t '.a l S U B J E C T T O P S O T E C T I V E c t3-DER* area . area. -- < firs t na x la s t peak nin . scan scan scan w idth raw area corr . area corr . Z 1 1 2.396 3 1 2.396 253 253 258 258 265 265 12 2 0 4 1 0 0 12 204100 169708 165892 10 0 . 0 0 9 7.7 5 - 321.9 'st p e a k i s b a s e l i n e . d r o p c o r r e c t e d a r e a , ond p e a k i s t a n g e n t s k i n n e d c o r r e c t e d a r e a . K R .T . f i r s t nin . scan 1 12.396 2 12.396 253 253 na x scan 258 258 la st scan peak w idth 264 264 11 11 raw area 49003 49 0 03 C10999 c or r . area co rr. -/. & 0 C Q 6 20590 18626 100 .00 9 0.4 6 OOT0 86000 L o s 5 Z / S Z- S T 0 z dS * 2 IS * e - i n m s ' nura ' s z - ' 9 s z \z\zz< n j OS SdS/Svl-OSI OSSS-dS* 3dlS f r 0 - m m s ' TM * 9 ' 0 3 - 9 ' I 13 TSS < * t ! J OS S i ^ E ^ t - O S I 0 3 d S ' a l i * 0 - in -in3 ' nure` 9 ' 8 3 - 9 ' 3 I 3 i e a < * ?j os s3^ ^ i-08i e s s s d s ' a t u s t> es-in - i n - ' nuj* 9 '3 - 9 M i s i c a c ^ n j nS d a Ta f x 1e header fron >B3 i2 1 3anp le ? 2UL U -3047 Od e r a t o r : R U Y rtS M ise ; STAB. SP2330 1 8 0 - 1 / 3 / 2 7 5 SCC BTL*53 BTL+S3 11/05/84 Svs . # : i MS M o d e l t 8 7 SW/ HW r e v . * CA A L S * : 0 h e t h od f i l e ; S P 2 3 3 0 Tuning f i l e : APEI01 No. of e x t r a re c o rd s- S o u rc e t e n p .; 250 Analyzer ten p . 0 T ra n s fe r lin e tenp . C h ro n a to g ra p h ic Ch.r ona t og r a p h i c Chronatographic tenperatures tin e s, n in . ra te > d e g /n in ; 0. 0 .0 0 . Cl 0. 0. 0 0.0 0. 0. 0 0.0 1D . 0. 0 0 .0 0. 0.0 0 .0 h/Z = 333.9 F i r s t deak is b a s e lin e d r op c o r r e c t e d a r e a . Second peak is tangent skinned c o rre c te d a r e a . Pea k t R .T. f ir s t Min . scan Ma x scan la s t scan peak w id th raw area i 12.355 2 12.355 252 252 256 256 265 265 13 168497 13 168497 corr . area 135802 131921 corr . V 1 00 . o 0 9 7 .1 4 h/Z - 3 3 i.9 F i r s t peak is b a s e lin e d r op c o r r e c t e d a r e a . Second peak i s tang ent sk in n e d c o r r e c t e d a r ea . Peak # R .T. ni n . fir s t scan 1 i 2 . 355 2 1 2 . 355 252 252 na x scan 256 256 la s t scan peak w id th 266 i4 11111 * 11 n 1W 1 1 raw area 148241 148241 corr . area 113409 110994 corr. X 100.00 9 7 . 37 332/334 CALCULATION R - G l o b a 1< 0 ) = .8351 ------ r - ______^ h/Z - 327.9 -1 7 T ~ r F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak is; tangent skinned c o rre c te d a re a . Peak # R .T. nin . fir s t scan na x scan la s t scan peak w id th ' raw area i 12.375 2 12.375 252 252 257 257 266 266 14 1 7 4 7 7 5 14 1 7 4 7 7 5 h/Z ~ "321.9 F i r s t peak i s b a s e lin e drop c o rre c te d area . Second peak is tangent skinned c o rre c te d area . Peak t R .T. f i r s t M in. scan na x scan la s t scan peak w id th raw area 1 12.37S 2 12.375 253 253 257 257 268 268 15 5 5 1 0 8 3 15 5 5 1 0 8 3 corr. area corr. / 137633 134434 100.00 97.68 C11002 corr. area 512623 5 0 i4 i8 0 corr . % 100.00 97.31 First peak is baseline drop corrected area. Second peak is tangent skinned corrected area. Peak * R .1 . f i r s t nin . scan nax scan la s t scan peak wid th raw area i 12.395 2 12.395 252 252 258 258 269 269 17 4 56590 17 456590 corr . area 414889 405853 corr . 7. 100.00 9 7 .8 2 20/322 CALCULATION R-Glob a 1( i ) .8093 h/2 = 2 57 .0 F i r s t peak i s b a s e lin e dr'op c o r r e c t e d a r e a . Second peak is tangent skinned c o rre c te d a re a . F^a k * R .T. f i r s t n in . scan na x scan la s t scan peak w id th raw area i 12.395 2 12.395 252 252 258 258 269 269 17 2 9 2 4 4 3 i 7 292443 corr . area 213527 216334 c or r . 100.00 99.00 <320 + 3 2 2 ) / < 3 3 2 + 3 3 4 ) CALCU LATIO N R -G Iob al< 3) = 3 .7 2 1 8 < 3 2 8 ')/ (3 3 2 + 334) CALCULATION R - G o b a I < 3 ) = .5338 <. C11003 F i l e > 3 1 2 2 3 3 3 . 6 - 3 3 - 4 . 6 illi 2 UL U T - 3 0 4 3 S T O B . S P 2 3 3 0 1 80 -1 ^ 3^ 27 5 SC F i l e >3122 3 2 1 . 6 - 3 2 2 . 6 itiu.SU L U T -3 0 4 8 S T A B .S P 2 3 3 0 180-1^3^-275 SC U5JECT TO ?RC T ^ T1i1V F** ORDER. C1100.4 hS da ta file header fron >B3 i22 Sano Xe = HL U r - 3 0 4 8 O p e ra to r: KY fiS l l /05/84 Mise ' S T A B .S P 2 3 3 0 1 3 0 - 1 / 3 / 2 7 5 SCC BTL*55 BTL*S5 S y s . ;i f : i H S Model: 8 7 SW/ HW r e u . : C A A L S * = Method f i l e : SP2330 tuning file .- APEIOi No. of e x t r a r e c o rd s - 2 S o u rc e t e n p .: 250 A nalyzer teMp. T ra n sfe r lin e tenp. 3 =4 5 U C h ro n a to g ra p h ic ChfTonatographic C h ro n a to g ra p h ic tenperatures t i n e s > nin . ra te , deg/nin: 0. 0. 0 .0 0. 0.0 0.0 0. 0.0 0.0 0. 0 .0 0 .0 0. 0. 0.0 h/Z = 333.9 f i r s t peak i s b a s e lin e drop c o rre c te d area . Second peak is tangent skinned c o rre c te d a r e a . Peak * R .T . f i r s t nin . scan i 12.355 2 2.355 252 252 nax la s t scan scan peak w id th 256 256 268 268 16 16 raw area 192609 92609 c or r . area 153953 150769 corr . 7. 100.00 97.93 H/Z - 3 31.9 F i r s t p e a k :i s b a s e l i n e d r op c o r r e c t e d a r e a . Secondi peak i s tangent skin n ed c o rre c te d a re a . Peak * K .T . firs t nin . scan na x scan la s t scan peak w id th raw area corr . area corr . / i 12.355 D 12.355 252 252 256 256 266 266 14 1 5 9 4 0 4 14 159404 124292 121688 10 0 . 0 0 97.90 332/334 CALCULATION R - G l o b a l < 0 ) = .8073 ri / 7. ~ 3 2 7 . S' F i r s t peak i s b a s e lin e drop c o rre c te d area . Second peak i s tangent skinned c o rre c te d are a . Pea 4F R .T. f i r s t nin . scan nax scan la s t scan peak w id th raw area 1 12.375 2 12.375 252 252 257 257 267 267- 15 1 8 9 0 6 3 iS 189083 ri/ Z i . 9 F i r s t peak i s b a s e lin e drop c o rre c te d area . Second peak is tangent skinned c o rre c te d a re a . Peak # R .T. f ir 51 nin . scan na x scan la s t scan peak w id th raw area 1 12.395 252 258 263 11 36775 2 12.395 252 258 263 11 36775 c or r . area 149138 145133 corr. 100.00 97.31 c or r . area corr . 9792 i 00 . 00 8934 91.24 C11005 h/ / 319. ? First peak is baseline drop corrected area. Second peak is tangent skinned corrected area. ak R .T . fir s t nin . scan i 12.395 2 12,. 3 9 5 255 255 nax scan 258 258 la s t scan peak w id th 262 262 7 7 raw area 25072 25072 7 0 2 i 2. Z. c or r . area 7138 6875 c o rr . /. 10 0 . 0 0 9 6 .3 2 320/322 CALCULATION R-G lobaI< i) = .7290 rt/Z = 2 5 7 .0 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak i s tangent skinned c o rre c te d a r e a . i-- C Peak # fir s t nin . scan na x scan la s t scan peak w id th raw area 1 12.395 2 12.395 256 256 258 258 262 262 6 27295 6 27295 corr . area 5905 5848 c orr . X 100 . 00 9 9 .0 3 (320 + 322)/< 332 +334) CALCULATION R- G l o b a I( 3) = .0608 < 328'> /(332 + 334) CALCULATION -G lo b ali 3) - .5357 'll u l C'- i p ip f r o rr>. ^ ` *- 2ER, V C11006 F i l e > B 3 1 2 3 333.6-334 r- s-fTi'J 2UL- UT.- 3 0 4 9 T A B . S P 2 3 3 0 2 0 O - 1 >'3^25 0 RUN F i l e >B3123 3 2 1 .6 - 3 2 2 .6 amu.SUL UT-3G49 S T A B . S P 2 3 3 0 2 0 0 - 1 ^ 3 ^ 2 5 0 RWH ----- f \ "i* U u l ! SUBJECT TO PROTECTIVE CRDR, C11007 rt v- rj 3 1 3 i- i, J.e h e 3 d e r r o n '8 3 1 2 3 'j a n g l e : 2 U L (J1 - 3 (J4 9 O p e r a t o r : ROY MS H i s c = S T A B . S P 2 3 3 0 2 0 Q - i / 3 / 2 S 0 RWN BTL*S7BTL*57 1 i / O S / 8 4 ^4 =ii S y s . = 1- i t S M o d e l i- 8 7 S U / H W r e v . C A A L S # ; 0 Method f i l e : SP2330 Tuning f i l e : APEIOi No. of e x t r a r e c o r d s : 2 So urce t e n p .; 250 Analyzer tenp .: 0 Tra n sfer lin e tenp. 0 Chronatographic tenper at ures Ch.ronatographic t i n e s , n i n . C h r o n a t o g r a p h i c r a t e j. d e g / n i n : 0. 0. 0.0 0. 0.0 0.0 0. 0.0 0.0 . 0.0 0.0 0. . 0 0.0 H/7 = 3 3 3 .9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s tangent skin n ed c o rre c te d a r e a . P e a i< * R .T . firs t nin . scan na x scan la s t scan peak w id th raw area i 12.354 12.354 250 250 256 256 272 272 22 206564 22 20 6564 corr . area 15.1916 149012 c or r . /u i 00.00 98.0 9 rt / l - 3 3 i . ? F i r s t peak i s b a s e lin e drop c o rre c te d area . Second peak is tangent skinned c o rre c te d a re a . Peak * R . T. fir s t nin . scan M3 X scan la s t scan peak w id th raw area i 12.354 ? 12.354 246 246 256 256 267 267 2 i i 73310 2 i 173310 corrV area 125136 i i979'i c orr . v 100 . 00 9 5 .7 3 332/334 CALCULATION R - G l obal-C 0) = . 8237 n/Z ~ 3 2 7 . 9 F i r s t pea k i s b a s e l i n e drop c o rre c te d a re a . Second peak is tangent skinned c o rre c te d a re a . S U B J t C T T OU rP'PRCT *Oc.? Peak 4 R .T. f i r s t nin . scan na x scan la s t scan peak w id th r a u! area c or r . area c orr . % 1 12.375 2 12.375 253 253 257 257 265 265 12 177485 145457 10 0.00 12 i 77485 i 41251 97 . i-l rt/'i - 3 2 i . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak is tangent sk in n e d c o rre c te d a re a . --1 Pea k * fir s t nin . scan i 12.375 ? 12.375 253 253 na x scan 257 257 la s t scan 264 264 peak w id th ii ii raw area 36003 363 C11008 Of N\'%}j* to) corr . area c orr . % 8151 7634 i 00 . 00 9 3 .6 6 5 ri/ 1 - 3 i 9 . V First pea is base'line drop corrected area . Second peak is tangent skinned corrected area. Peak * R .T. f i r s t nin . scan i 12.375 2 12.375 254 254 nax scan 257 257 la s t scan 265 265 peak w id th ii ii raw area 34404 34404 ^ 631 ? 3 corr . area 7014 6865 corr . /m 10 0 . 00 9 7 . 88 320/322 CALCULATION , R-G lobali i) = .8605 h/Z - 257.0 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak i s tangent skin n ed c o rre c te d a r e a . Peak # K .T. f i r s t nin . scan nax scan la s t scan peak w id th raw area 1 12.536 26 i 265 272 ii 42210 2 1 2 . 5 3 6 2 6 i 2 6 5 2 7 2 11 4 2 2 1 0 corr . area 4040 3308 corr . /. 100 . 00 3 1 .3 8 <320 + 2 2 ) 7 ( 3 3 2 + 3 3 4 ) C A LC U LA T IO N R-Global< 3) = .0547 < 3 28')/< 332 + 334) CALCULATION R-Global( 3) = .5248 SU: CCf nr C11009 fil* >B3124 333.6-'334.6 amu .*UL U T - 3050 STflB.3P2330- 3O0-1/3/250 RUM file >E3124 321.6-322.6 -a.mu.2UL UT-3050 STflB .SP2330 200-1/3/250 RUM cuoio "! 'I t -i f i L e h f' : ci e r i' r n n 5l2'4 *. 5 n [) i ' p j i Vi I ) I -j 5 0 O p e r a t o r - H Y M'a L i / `i 5 / H4 Mise S F A B . S P 2 3 3 0 0 0 - 1 / 3 / 2 5 0 RUN B f L 5 9 B T L +5 ? S MS . fc i fib n o d e ! ; h e t h od f i l e t S P 2 3 3 0 3 / S U / H U r e v . CA A L S it 0 T u n i n g f i l e * A F L I 01 N o . o f e x t r a ir e c o r d s S o u rce t e n p .; 250 Analuzer tenp . ? G T r a n s f e r l i n e t enp . C h ro n a to g ra p h ic C h ro n a to g ra p h ic C h ro n a to g ra p h ic tenperatures . t ines n in . r a t e * deg/ni.n= 0. 0.0 0.0i 0. 0 .0 0 .0 0. 0.0 0 .0 0. 0.0 0. 0. 0.u 0.0 -i - 2 5 fir5 " 333.7 ' F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak is tangen t skinned c o rre c te d area . Pe a k # R . 1. first run . scan nax la s t scan . scan peak w id th raw area i 12.368 2 12.368 255 255 260 260 272 272 17 1 7 1 2 4 6 17 191246 corr . area 143933 14577? c or r . /to 10 0 . 00 * 7 . 83 i t / z = 5 3 1 . ? F i r s t peak i s b a s e lin e drop c o rre c te d area . Second peak i s tangen t sk in n e d c o rre c te d a re a . Pea K 4 R .T. mi n . f irst scan i 12.368 2 12.363 254 54 nax scan 260 260 la s t scan peak w id th 271 271 17 17 raw area 163470 163470 c or r . area 122432 119117 c or r . tm 100.00 7 7 . 2? *VrT 534 CALCULATION fi-Giobal< 0) = .8221 h // - 527 9 F i r s t peak i s b a s e lin e drop c o rre c te d area Second peak i s tangent skin n ed c o rre c te d are a err U e ^ c r -i OC ;P C . i Pea k * R .T. f i r s t nin . scan na x scan la s t scan peak w id th raw area corr . area c or r . X 1 12.30? c_ 1 2 . 3 8 9 H/ Z " 3 8 1 . 7 257 257 261 261 268 268 11 177'366 145587 10 0 . 0 0 11 177366 i 4i 511 77.20 F i r s t peak i s ! ba s e 1 i ne d r op c o r r e c t e d a r e a . Second peak i s tangent skinned c o rre c te d area . Peak * R.T . firs t nin . scan nax scan la s t scan peak w id th raw area 1 12.38? 256 261 269 13 46073 2 12.389 2S6 6 i 269 13 46 073 corr . area corr1. V 13833 13027 100 00 94.17 C11011 \ rl ->: " .71 'v . 9 P i r -r.t p e a k i s b a s e l i n e drop c o rre c te d area . b e e one! p e a k i s t a n g e n t s k i n r i e d c o r r e c t e d a r e a . Peak t R .T . n in . firs t scan nax scan la st scan peak w idth raw area i 1 2.389 2 12.389 258 258 261 261 267 267 9 34662 9 34662 '7 3 j 7 'f corr . area 11163 10803 corr . /L 100.00 9 6.7 8 3 2 0 /3 2 2 CALCULATION R - G `1 ob a I < 1 ) .8070 - ri '*/ = 2 5 7 . 0 Fr i r s t p e a k i s b a s e l i n e d r d c o r r e c t ed a r e a . Second peak i s ta n g e n t skiMMed c o r r e c t e d a r ea . Peak * k .1 . first M in. scan na x scan la st scan peak w id th raw area i 1 2.339 257 261 267 10 46154 2 , 12.389 257 261 267 10 46134 corr . area 1 0304 10 20 9 corr . Vtm 10 0 0 0 99.0 8 < 320 + 3 2 2 ) / < 3 3 2 + 3 3 4 ) CALCULATION R -G lo b a K 3) - . 0921 `23' )/<332 + 334) CALCULATION R-Global( 3) - .5360 SLBJECT t TC7,7 ? ^ J /N o , C11012 8TOITO O K ir lj vy 13 71 3 O S ^ S / I - O O ? . 0 c d S 03- /'S* ` SO * 0 T "i r i c ` nui ' S S - ' 9 S S S S I a < * U J IS 13 0SS/'^T-003 0c dS 0 3 */8fr*/SO' 0 i r i S ' n^ 9 ' 0 S - 9 ' 6 I SSIES< S I ? J la 1 3 0S 3^ / T -003 0 3 d S 0 3 ' / 8 t , ' / ' 0 ' 0 T " i n s ' nul* S ' S S E - S ' I S E S S T 3 < S I T J l a 1 3 0 5 3 / ' / t - 0 0 S 0 3 d S 0 3 ' /* * / S O ' G I " i n s ' nure ? * 8 3 - 9 ' 3 S 3 T 3 < * I ! J ia i s 05S / 8/ I - 00C 0cds 0 3 ' / s ^ * / 3 0 * 0 T " i n s ' nure S 'Z t Z ~ ? 'X t Z S t i e a ^ ^ I T J iVi d a t a ' t i l e h e a d e r f r o n = > B 3 1 2 5 S a m p l e ; 2UL it) . 0 2 / . 4 8 / . 20 ( J p e r a t o r ; ROY h i s c = 8 P2330 2 0 0 - 1 / 3 / 2 5 0 GT BTL417 BTL417 rIS ll/O S /3 4 4-47 Svs. * i h S - n o d e l : 87 SW/HU r e v . - CA ALS * . 0 M e t h o d f i l e * . SP2330 Tuning file-- APEI01 No. of e x t r a r e c o r d s ; Source tenp.-. 248 Analyzer tenp.i 0 T ra n sfe r lin e tenp. 0 Ghronatographic tenp eratures : Chronato araph ic t i n e s , nin . G Mr o n a t o g r a p h i c r a t e ^ d e g / n i n 0. 0.0 0.0 0. 0.0 0.0 0. 0 .0 0 .0 0. 0.0 0. 0 0. .0 . 0 N/I - 333.9 F i r s t peak i s b a s e lin e d r op c o r r e c t e d a r e a . Second peak is; tangent skinned c o rre c te d area . Peak * R .T. f i r s t nin . scan na x scan la s t scan pea k w id th raw area corr . area corr. X i 12.375 2 12.375 250 250 257 257 268 268 18 424578 380406 100 . 0Q 18 424578 376518 9 8 .9 8 h /I - 331.9 F i r s t peak is b a s e lin e drop c o rre c te d area , Second peak is i tangent sk in n e d c o rre c te d are a . Pea k 4 R .T . firs t nin . scan na x scan la s t scan peak w id th raw area i 12.375 2 12.375 252 252 257 257 267 267 15 352807 15 352807 corr . area 314857 311812 corr . X 100.00 9 9 .0 3 32/334 CALCULATION R-Gl oba 1< 0> - .8277 n //. - 3 2 7 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d area . Second peak i s tangent skin n ed c o rre c te d are a . Peak 4 R .T. f i r s t nin . scan nax scan la s t scan peak w id th raw area i 12.395 4O_ 1 2 . 3 9 5 250 250 258 258 268 268- 18 18 522373 522373 H/Z = 3 2 1 .9 F i r s t peak i s b a s e lin e drop c o rre c te d area . Secondi peak i s tangent sk in n e d c o rre c te d a r e a . Peak * K .1 . f i r s t nin . scan na x scan la s t scan peak w id th raw area i 12.395 2 12.395 252 252 258 258 270 270 18 7 5 7 2 8 9 0 13' T ^172890 corr. area 475141 468535 corr. 100.00 93.61 O J.JLU J.3r c o rr. area 7529474 7443425 corr . % 100.00 9 8 .8 6 Vj n^'Z - 3l9.9 F i r s t peak i s b a s e lin e drop c o rre c te d a re a . Second peak is tangent skinned c o rre c te d a re a . Pea k * R.T . firs t nin . scan na x . l a s t scan scan peak w id th raw area 1 12.415 2 V i . 415 253 253 259 259 274 274 21 6 226951 21 6226951 corr . area 6175942 6118413 corr . X 100.00 99.0 7 320/322 CALCULATION R-Globa1< 1) = .8202 h/Z = 257.0 First peak is baseline drop cor rec ted area . Second peak is tangent skinned corrected area . Pea l< I- K .T . first na x last peak nin . scan scan scan width raw area 1 12.415 253 259 279 26 3075655 i-- 12.415* 253 259 279 * 26 3075655 corr. area 2991051 2968600 corr. X 100.00 99.25 <320 + 3 2 2 > / i3 3 2 +334)' CALCULATION R-Glo b a 1 C 3 ) = 1 9 .7 1 2 b <320')/<332 + 334) CALCULATION R-Giobal( 3) - .5859 I *** -'f-'-C'b ^ ^ ,j r> C11015 File >B 3 16 333.6-334.6 arr.u.2UL UT-3051 ST A B .SP2330 200-1/3/2E0 RUN F i l e > 3 1 2 6 3 2 1 . 6 - 3 2 2 . 6 atriu.^UL U T - 3 9 5 1 S T R B . S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN JL hA .j, ", . . A --Led J3JECT t o p r o t o c t v ; : : r o e r . osM C lio 16 ni - a a t a f i l e h e a d e r f r o M ; >B 3 i 2 6 SsMple: 2 U L U T - 3 Q S Operator; k.OY MS 11/05/84 5 i 0 M i s e ; S T A B . S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN BTL#63BTL#63 3 vs . * i i MS Model: 8 7 S U / H U rev.: C A A L S # = 0 Method f i l e : SP2330 Tuning f i l e : APEIQi No. of e x t r a r e c o r d s - 2 So u rce t e n p .; 250 Analyzer te n p . 0 T r a n s f e r lin e tenp,. 0 C h ro n a to g ra p h ic ^C h r ona t o a r a p h i c C h ro n a to g ra p h ic tenperatures tines t nm . ra te , deg/nin: 0. 0.0 0.0 0. 0.0 0.0 0. 0.0 0. 0 0. 0.0 0.0 0. 0.. 0 0 .0 rl/2 = 3 3 3 . ? F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak is tangent skinned c o rre c te d a re a . Pea k * k.T. f ir s t nin . scan i 12.355 2 12.353 251 251 na x scan 256 256 la s t scan peak w id th 265 265 14 i4 raw area 134268 134268 corr . area 100360 95915 c or r . X i 00 . 00 9 5 .5 7 M/Z - 3 3 i . 9 f i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tangent skin n ed c o rre c te d a r e a . Peak * K -T. f i r s t nin . scan i 12.375 `3_ 1 2 . 3 7 5 253 253 na x scan 257 257 la s t scan 267 267 peak w id th 14 14 raw area 120926 120926 corr . area 837 0 0 82496 corr . V Ml i 00.0 0 9 3 .5 6 332/53** CALCULATION R - G io b a l( 0) = .8340 ri//. " 3 2 7 . 9 F i r s t peak is b a s e lin e .drop c o rre c te d area. Second peak i s tangent skin n ed c o rre c te d a r e a . Peak * k.T. f ir s t nin . scan na x scan la s t scan peak w id th raw area i 12.396 3 1 2 . 3 9 6 253 253 258 258 266 266 13 138628 13 138628 n/Z - 321.9 F i r s t -peak i s b a s e lin e drop c o rre c te d are a . Second peak is tangent skin n e d c o rre c te d a r e a . Peak t k .T . f ir s t nin . scan i 1 2.396 1 2 .3 9 6 253 253 na x scan 253 258 la st scan 268 268 peak w idth 15 15 raw area 74495 74495 AT \ 54 ^-j" ,,w rxI H. corr . a rea :i 0 4 7 2 4 101357 c orr . X i 00 . 00 96.78 C11017 c orr . area 3635 3542 0 corr . V/% 10 0 . 00 9 7.4 4 ri / Z = 5 i 9 . 9 f i r s t peak is b a s e lin e drop c o rre c te d a r e a . Second peak i s tangent sk in n e d c o rre c te d a r e a . Peak t K .T . fir s t nin . scan nax scan la s t scan peak w id th raw area i 12.396 O 12.396 253 253 258 258 266 266 13 61532 13 61532 ^ 3 ( 2-U corr. are a 27784 27576 corr. 1 00.00 9V . 25 '320/322 CALCULATION R - G lo b a l( 1) - .7643 I'i / /_ -- 2 5 ? . 0 F i r s t peaK i s b a s e lin e drop c o rre c te d are a . Second peak is tangent skinned c o rre c te d a re a . Peak * K -T. f i r s t nin . scan 1 12.396 2 12.396 253 253 na x scan 258 258 la s t scan pea k w id th 264 264 li 11 raw area 54128 54128 corr . area corr. a*y 17421 i 00 . 00 15303 87.84 i .320 + 3 2 2 > / < 3 3 2 + 3 3 4 ) C A L C U L A T I O N R - C lo b a l( 3) - .3484 :32B/ )/< 3 3 2 + 3 34 ) CALCULATION R - G ' i o b a l C 3 ) = .5672 C11018 e >B3 127 3 3 3 . 6 - 3 3 4 . 6 a m u .^ U L U T - 3 0 5 2 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 PUH BT 15/64 5:'29 r is ii 0. (1. 0 0.0 rr . 1.00 . 03 e >B 3 17 3 2 1 . 6 - 3 2 2 . 6 amu.2UI_ U T - 3 0 5 2 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RWN B T rr . 7 . 00 . 16 C11019 X .00 04 * r. 00 85 <0 00 CD W i> ri/7. = 3 l 9 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s tangent skin n ed c o rre c te d a r e a . Peak * H.T . f ir s t nin . scan na x scan la s t scan pea k w id th raw area i 12.395 2 12^ 3 9 5 255 255 258 258 266 266 .11 11 88479 88479 T' t l l ' i ' L ' l corr . area 59021 58328 corr . X 100.00 320/322 CALCULATION R - G l o b a I ( 1 ) = .7939 ri/Z = 2 5 7 .0 F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak i s tangen t skinned c o rre c te d area . Peak K .T . firs t nin . scan na x scan la s t scan pea k w id th raw area i 12.395 2 i 2.395 252 252 258 258 265 265 13 13 77888 77888 (320 + 3 2 2 )/ ( 3 3 2 +334) CALCULATION R-GlobaH 3) = .4940 ' corr . area 34156 33506 corr' . 100.00 98.10 (3 2 8 ')/ < 3 3 2 + 334) CALCULATION R -G lobaK 3 > = .5416 n cy* C11021 Fi U >B3128 333.6-334.6 amu.SUL UT-3053 SP233Q 200-1/3/250 RUN BT F i l e >B3128 3 2 1 .6 - 3 2 2 .6 amu. S U L .UT-3053 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 S 0 RUN BT C11022 MS d a t a f i l e h e a d e r f r o m : > B 3 1 2 8 Sam ple: 2UL UT-30S3 O p e r a t o r : ROY MS 11/05/84 .5:4 9 M i s c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN B T L 4 6 7 B T L # 6 7 Sys. 1 MS m o d e l : 8 7 SU/HW r e u . : Cfl R L S # : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 No. o f e x t r a r e c o r d s : 2 Source tem p .: 250 R n a ly ze r tem p .: 0 T r a n s fe r lin e temp. : 0 Chromatographi c tem peratures : 0. 0. 0. 0. 0. Ch r o ma t o g r ap h i c t i m e s , m i n . : 0 . 0 0 .0 0. 0 0 .0 0. 0 Chromatographi c ra te , deg/min: 0 .0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d area . Sec ond peak i s t angent skimmed c o r r e c t e d a r e a . Peak R .T. min. fi rst scan max scan 1a s t scan peak w id th raw area co rr. area co rr, y. 1 12.355 2 12.355 250 250 256 256 266 266 16 2 0 8 6 0 9 16 2 0 8 6 0 9 166849 162753 100.00 97.55 M/Z = 3 3 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak i s tan g e n t skimmed c o r r e c t e d a r e a . Peak # R .T . min. fi rst sc an max scan 1a s t peak sc an w id t h raw area c or r . area corn. *4 1 1 2 . 3 5 5 2 48 25,6 268 12.355 243 256 268 20 191713 137753 100.00 20 191713 135873 98.64 332/334 CRLCULRTION R -G lo b aK 0) = . 8256 M/Z = 3 2 7 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak i s t angent skimmed c o r r e c te d a re a . Peak # R .T . min. f i rst sc an max scan 1a s t peak sc an w id t h raw area 1 12.375 2 12.375 252 252 257 v 267 257 267 15 2 0 S 4 6 3 15 2 0 S 4 6 3 M/Z = 3 2 1 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d ar ea . Sec ond peak i s t angent skimmed c o r r e c t e d a r e a . Peak # R .T . min. f i rst sc an max scan 1a s t scan peak w id th raw area 1 12.375 2 12.375 - .. - ' 255 255 . 257 257 . '7 'Ju 260 260 5 5 O n/ 22714 22714 cor r . ar ea 164288 162443 co rr. * 100.00 98.88 co rr. area 7064 7046 co rr. V. 100.00 99.75 C11023 s M/Z = 319.9 F i r s t p e a k i s' b a s e l i n e drop c o rre c te d are a . Second peak i s tang en t skimmed c o r r e c te d a re a . Peak # R .T . min. fi rst s c an max scan 1as t peak scan `width raw area i .12.375 2 '12.375 251 . 251 257 257 264 264 13 4 2215 13 4 2 2 1 5 ^ B 3 iZ S > co rr. area 8896 8636 corn. y 100.00 9 7 .0 8 320/322 CALCULATION R -G 1o b a l ( 1) = 1.2593 M/Z = 2 5 7 . 0 F i r s t peak i s b a s e l i ne drop c o rre c te d a re a . Second peak i s tang en t skimmed c o r r e c te d a re a . Peak # R .T. min. f i rst scan max scan 1a s t scan peak w id th raw area 1 12.375 2 12.375 252 252 257 257 263 263 11 4 6 0 6 4 11 4 6 0 6 4 co rr. area 8719 8526 c o rr. y. 100.00 9 7 .7 9 (320 + 3 2 2 )/ (3 3 2 +334) CALCULATION R-G lobal( 3) = .0524 ( 3 2 8 0 / ( 3 3 2 + 334) CALCULATION R -G lo b al( 3) = .5391 0121 C11024 F ile >3129 333.6-334.6 amu.SUL UT-3054 SP2330 200-1/3/250 RUN IT 40000- 20000- -1 7 "7-1 - 1 -1 -1-i--r~ i--r~ ;--i T 'it p i t i * i * i*r T T T *r * n ----r r p r r n "[ t t i ~ i ~) - r ~t ~ r --j --i --i | 10.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 15.6 F i l e >3129 3 3 1 .6 - 3 3 2 .6 amu.SUL UT-3054 S P 2 3 3 0 2 0 6 - 1 / 3 / 2 5 0 RUN T F i l e >3129 3 2 1 .6 - 3 2 2 .6 atnu.2UL UT-3054 S P 2 3 3 2 0 0 - 1 / 3 / 2 5 0 RWH B T 4000-1 2000n 0-(- 1ii-1- i 10.0 10.5 VE ORDER. irp r"i*i*r f r^T r | i-rr-r-^-rrrr i-i i-i-j- i--r-^ t n t i 11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 OO . A. ; C11025 15'.0 MS d a t a f i l e h e a d e r f r o m i > B 3 1 2 9 Sample* 2UL UT-3054 O p e r a t o r : ROY MS 11/05/84 Mi s c i S P 2 3 3 8 2 0 0 - 1 / 3 / 2 5 0 RUN B T L 4 6 9 B T L # 6 9 S y s . #* 1 MS m o d e l : 8 7 SU /H U r e v . : CA R L S # : 0 Method f i l e : SP2330 Tuning f i l e : RPEI01 No. o f e x t r a r e c o r d s : Source tem p .: 250 A n a ly z e r tem p.: 0 T r a n s f e r lin e temp. : e -Chromtographi c tem peratures : 0. 0. 0. 0. 0. Chrom atographic t i mes, min. : 0 .0 0 .0 ' 0 .0 0 .0 0 .0 Chromtographi c ra te , deg/min: 0 .0 0 .0 0 .0 0 .0 0 .0 M/Z * 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tang en t skimmed c o r r e c t e d ta r e a . Peak * R .T. min. fi rst scan max scan 1a s t peak s c a n wi d t h raw area com . area co rr. X 1 12.355 2 12.355 252 252 256 256 270 270 18 186388 142756 100.00 18 186388 139030 9 7 . 3 9 M/Z " 3 3 1 . 9 F i r s t peak t s b a s e l i ne drop c o rre c te d a re a . Second peak i s tangent skimmed c o rre c te d a r e a . Peak # R .T. min. f i rst scan max sc an 1a s t peak sc an w id th raw area c o rr. area c o rr. x - 1 12.355 252 256 268 2 12.355 252 256 268 16 155143 117207 100.00 16 155143 113935 9 7 .2 1 332/334 CALCULATION R-GIobalC 0) = .8 2 1 0 M/Z = 3 2 7 . 9 F i r s t peak i s b a s e lin e drop c o r r e c te d .a r e a . Second peak i s tang en t skimmed c o r r e c te d a r e a . Peak # R .T. min. fi rst sc an max scan 1a st peak scan width raw area corr. area co rr. X 1 12.375 245 257 269 2 12.375 245 257 269 24 204193 132505 100.00 24 204193 132193 9 9 .7 6 M/Z = 3 2 1 .9 F i r s t peak i s base lin e drop c o rre c te d a r e a . Sec ond peak i s t a rg e n t skimmed c o r r e c t e d a r e a . Peak # R .T. min. fi rst scan max sc an 1as t peak sc an w id t h raw area co rr. area co rr. 1 12.395 2 12.395 255 255 258 258 262 262 CS* j , .-t J. A * SU B JEC T TO PROTECT iV F O R n rp 7 26293 7 26293 7995 7288 nn - AJ C11026 100.00 9 1 . 16 S M/Z = 319.9 F i r s t peak i s base 1 i ne drop c o r r e c t ed a r e a . Sec ond peak i s t angent skimmed c o r r e c t e d a r e a . Peak ft R .T . min. fi rst scan max sc an 1a s t peak sc an u i dt h r aui area 1 r 1 2 .3 9 5 254 258 271 2 1 2 .3 9 5 254 258 271 17 5 0 7 1 0 17 5 0 7 1 0 > 63 co rr. area 9468 9417 c o rr. Ji 100.00 9 9 .4 6 3 2 0 / 3 2 2 C fL C U L fT ION R - G lo b a l< 1) = 1.1842 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s tan g en t skimmed c o r r e c te d a r e a . Peak ft R .T. min. fi rst scan max scan 1a s t peak scan ui dth raw area 1 0.808 2 0.000 272 272 0 271 0 ' 271 -1 -1 0 0 co rr. area 3897 3897 corr. y. 100.00 100.00 ( 3 2 0 + 3 2 2 > / < 3 3 2 + 3 3 4 ) C f L C U L f T I ON R -G lo b al< 3) .0672 ( 3 2 8 ' >/<332 + 334) CALCULATION R -G lo b al< 3) = .5094 T t ` L-d OT!ZC j IV *j R .R, ^ ^ 4^ A ' * C11027 File >E313O 3 33.6". i-1 i t .affiu ^ UT-3055 SP233G 2GG-1/3/250 RUN ET F i l e >E 3 1 3 G 3 2 1 . 6 6 affi u 2UL U T - 3 0 5 5 S P 2 3 3 0 2 O 0 - 1 / 3 / 2 5 0 RUN BT MS data file header from : >B3130 Sam ple: 2UL UT-3055 O p e r a t o r : ROY MS 11/05/84 M i s c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN B T L # 7 1 B T L # 7 1 Sys. #: 1 MS m o d e l : 8 7 SW/HU r e v . : Cfl A L S # : 0 Method f i l e : SP2330 Tuning f i l e : APEI01 No. o f e x t r a r e c o r d s : 2 Source tem p .: 250 A nalyzer tem p.: 0 T ra n s fe r lin e temp. : 6 :.29 CD Chromtographi c t emperat ures : 0. 0. 0. >C h r o m t o g r a p h i c t i m e s , m i n . : 0 . 0 0 . 0 0 . 0 0 . 0 0 . 0 C h r odia t o g r a p h i c r a t e , d e g / m i n : 0 . 0 0 . 0 0 . 0 0 . e 0 . 0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area. Second peak is tangent skimmed c o rre c te d a re a . Peak It R .T. min. firs t s c an max scan la s t peak scan u i dth raw area co rr. area c o rr. y. 1 1 2 .3 7 5 251 257 269 2 1 2 .3 7 5 251 257 269 18 199421 18 199421 152945 149318 100.00 9 7 .6 3 M/Z = 3 3 1 . 9 ' Fi r s t peak is b a s e lin e drop c o rre c te d area. Second peak is tangent skimmed c o rre c te d a re a . Peak # R .T. min. fi rst s c an max scan 1a s t scan peak w id th raw area c o rr. area co rr. % 1 1 2 .3 7 5 251 257 268 1 2 .3 7 5 251 257 268 17 169442 127707 100.00 17 169 4 42 1 2 4 0 0 9 9 7 . 10 332/334 CALCULATION R-Global< 0) = .8350 M/Z = 3 2 7 . 8 F i r s t p e ak i s b a s e l i n e drop c o rre c te d area. Second peak i s tangent skimmed c o rre c te d a re a . Peak It R .T. min. f irst scan max sc an 1a s t peak scan width raw area 1 12.395 252 258 269 2 12.395 252 258 269 17 2 0 7 8 8 0 17 2 0 7 8 8 0 M/Z = 3 2 1 . 9 F i r s t peak i s base 1 i ne drop c o r r e c t ed a r e a . Sec ond peak i s t a n g e n t skimm ed c o r r e c t e d a r e a . Peak It R.T. fi rst mi n . s c an max sc an 1a s t peak sc an w id th raw area 1 12.395 2 12.395 `U*it ; . . SUBJECT TO 253 253 274 253 258 274 21 21 r\ o i 2 S )TtCr: ,E ORDER 670010 670010 co rr. area 159737 155741 c o rr. y. 100.00 9 7 .4 7 co rr. ar ea 618539 607409 corr. 100.00 9 8 .2 0 C11029 r-W = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. R. T. min. f irst scan max sc an 1a s t peak sc an w id th raw area r 12.395 252 258 288 12.395 252 258 268 16 5 5 4 3 8 4 16 554 3 84 S 3 i B Cj co rr. area 513920 560472 corr. Ji 100.00 9 7 .3 8 320^322 CALCULATION R - G lo b a K 1) = .8309 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak is tangent skimmed c o r r e c te d a re a . Pe ak * R .T . min. f i rst scan max sc an 1a s t peak scan width raw area 1 1 2 .3 9 5 251 258 271 2 1 2 .3 9 5 251 258 271 20 364735 20 364735 c o rr. area 290935 285515 c o rr. '4 100.00 9 8 . 14 C3 2 0 + 3 2 2 > ^ C 3 3 2 +3 3 4 ) C A L C U L A T I O N R -G lo b al< 3) = 4.0351 <328/ >/<332 + 334) CALCULATION R -G lo b ali 3) * .5495 i-' . SUBJECT TO P-HOTI-. A r' IT C11030 File >3131 3 .6-3 3 4 . 6 a m u .2UL .2504/. 43/. 20 SP2330 260-1/3/250 GT BT F i l e > 5 3 1 3 1 3 2 1 . 6 - 3 2 2 . 6 a m u . S U L . 2 5 0 4 / . 4 3 / . 20 S P 2 3 3 0 2 0 G - 1 / 3 / 2 5 0 GT BT riS d a t a f i l e h e a d e r f r o m : >S 3 1 3 1 Sam ple: 2UL . 2 5 6 4 /. 4 8 / . 20 O p e r a t o r : ROY MS 11/05/34 6 : 5 2 ' M ise : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL#29 BTL#29 Sys. #: 1 MS m o d e l : 8 7 SW/HW r e v . : Cfi R L S * : 0 M e th o d 'file : SP2330 Tuning f i l e : RPEI01 No. o f e x t r a r e c o r d s : 2 Source tem p.: 248 A nalyzer tem p.: 0 T ra n s fe r lin e temp. : 0 Chromatographi c tem peratures : Chromatograph i c t i mes, min. : Chrornatographi c ra te , deg/min: 0. 0 .0 0 .0 0. 0 .0 0. 0 0. 0 .0 0 .0 0. 0 .0 0.0 ' 0. 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tangen t skimmed c o r r e c te d a re a . Peak # R. T. min. fi rst sc an 1 12.376 o 12.376 250 250 max sc an 257 257 1a s t peak scan width 270 270 20 20 raw area 524902 524902 c o rr. area 470402 461832 c o rr. i: 100.00 9 8 . 18 M/Z = 3 3 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area. Second peak is tangent skimmed c o rre c te d a re a . Peak it R .T. min. firs t sc an 1 12.376 2 12.376 252 252 max sc an 257 257 1a s t peak sc an w id th 271 19 271 19 raw area 433748 433748 c o rr. area 384082 379313 corr. * 100.00 98.76 - _ * 332/334 CALCULATION R -G lo b al< 8) = . 8165 M/Z = 3 2 7 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak is tangent skimmed c o rre c te d a re a . *P e a k R .T . min. fi rst scan max sc an 1a s t scan peak w id th raw area 1 1 2 .3 9 6 252 258 271 2 1 2 .3 9 6 252 258 271 19 5 5G 359 19 550 3 59 M/2 = 3 2 1 . 9 F i r s t peak is b a s e lin e drop co rre c te d area. Second peak is tangent skimmed c o rre c te d a re a . Peak # inR . T . m. firs t sc an max sc an 1as t peak scan width raw area 1 12.396 2 12.396 . *_ 252 252 ,, .. -* -1 253 275 253 275 T'"T \ s __> L J 23 303091 23 303091 ft r i* r<y SU B JEC T TO co rr. area 492295 484552 co rr. * 160.00 93.43 co rr. area co rr. `4 246281 241037 100.00 9 7 .8 7 C11032 C1/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak # R .T. min. f irst s c an max sc an 1a s t peak scan width rau area 1 1 2 .3 9 6 25G 258 274 2 12.396 250 258 274 24 275452 24 275452 ^ Q 3 I3 I corr ; area 214564 212416 c o rr. * 100.00 99.00 320/322 CALCULATION R-GlobalC 1) = .8712 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak i s tan g en t skimmed c o r r e c te d a re a . Peak # R .T . min. fi rst scan max scan 1a s t peak scan width raw area 1 12.396 2 12.396 53 253 258 258 269 269 16 - 16 174909 174909 c o rr. area co rr. y. 116653 100.00 112437 96.39 (320 + 322) / (332 +334) CALCULATION R -G lo b aK 3) .5393 < 3 2 8 0 / (3 3 2 + 334) CALCULATION R -G lo b al( 3) = .5735 i\ : SLtiJts-i io 1c . \ 1 R . n n i 7r\ C11033 ri le- >B3132 6-334.6 affiu ,2UL UT-'3056 SP233Q 200-1/3/250 RUM ET File >33132 321.6-322.6 =litiu.2UL UT-3056 SP2330 2Q0-1/3/250 RUN ET mC cat a I? q Q h r t r e n : >33 *32 2 amp 1e * 2 UL ! J : - :>05b `O p e r a t o r : AY MS 11/05/34 N - s c ; S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RWN 3 T l - 75 B T l * 7 5 $ys. 1 MS m o d e l : 37 SW/HW r e v . : CA A L S ~ Method f i l e : SP2330 Tuning f i l e : API01 Source tem p.; 250 A n a ly ze r tem p.: 0 No. of e x t r a r e c o r d s : T r a n s f e r l i n e temp,, ; Chromatographic tem peratures : Chromatographic tin e s , mm. : Chromatographic ra te , deg/nin: nv - 0.0 0.0 C. 0.0 0.0 0. 0.0 0.0 0. 0.0 0.0 G. 0.0 0.0 M/Z - 3 3 3 . 9 i r s t peak is e a se l m e crop co rre c te d a re a . Second peal: i s tangent sKimmec c o rre c te d a re a . Peak R.7. f i r s t min. scan nax scan *y- c jw- o e a x s c a n tj l c t h r au area 1 2.375 9 ' 2.375 252 9c; ^ 257 257 270 270 13 203827 3 203827 cor r . area 1 5 5 " *! Q 152275 c o trr . a *0 0 . 0 0 98.17 M/Z = 3 3 1 . 3 7 : r 5 r peak ; s c a s e iin e crop co rrected area. Second pea* i s tangent skimmed c o rre c te c a re a . - eak * 9 5. : . mm . 12.375 12,375 f irs i scan 250 250 nax scan 257 257 la s t scan 270 270 p e aie width , 20 20 r au area P1 0 C | ^ 2 ' 80942 co rr. area 1 30522 126722 co rr. a. iOH. 0 0 97.09 7 ; 14 232/334 CALCULATION R -G local( 0 ) = .8 4 '4 M/Z = 3 2 7 . 3 peak is e a se l m e drop c o rre c te c area. Second peak i s tangent skimmed c o rre c te d a re a . peax 3 .7 . f ir s t min. scan nax scar. l a s t peak scan width rau area 1 1 2.395 9 i 2.395 M/Z = 3 2 1 _ c 252 252 258 258 270 270 213 2 2 3 9 3 5 i 223935 " i r s : peak i s b a s e ! i ne drop c o r r e c t e c a r e a . Second peak i s ta n g e n t sk immec c o r r e c t e c a r e a . Peak r- A. T. firs t min. scan max scan i a s z oea.< scan width r j ar--a A '!*-i s-i'-"* 1 ^ O O O 32- SUBJECT TO PROTECTIVE ORDER. co rr, area '70043 ' 63837 c o<r*r . A 100.00 86.33 corr . area corr . 7, C11035 OCA c;: nUl r .. !H o r J r- j o ~\> l o- i MI n lT) i (> lrA! PI F* L .5 -4 10 C11036 f I \ J -- - --. ro ro tu (OtO cn< _n fj r cLDn t(/J11 rj (.n hijij 00 rn ro r j aioi fo ro "vi --J foro coco c.n cn (Xi co 00 -- ' cooo -Vi i 3 \ co VJCT U lo <Z>I--i CO (-J> \ Gi oo M ^ 6 3 1.3 2 : r ifs: peak, is vaseline crop cor reeled area. Second peal; is tangent skimmed corrected area, Dear. R.. min. - !2 . 4 5 ~) 1 2 . 4 ! 5 fir s t scan 25 & 256 max scan 25S 259 l a s t peak scan ul dt h 268 268 12 19 rau area 40070 40070 cor: . area 8990 8492 co rr. X 1 0 0 . GO 94.4 G :2 0 /3 2 2 CALCULATION R-GIoDal( "> = .7599 'i/2 = 257.0 r 1 r s t oeaii i s D a s e i m e drop c o r r e c t e d a r e a . Second pea* is tangent skimmed c o rre c te d a re a . Dea< *Hv #T 4 17:1T . tri r s t scan max scan i a s t Deak scan u i dt h rau area 1 2.4:5 254 259 266 2 2 . 4 ' 5 2 5 4 2 5 9 &D 4 ^ 54041 tL. 54 04 1 co rr. area 778 : 7553 co rr. X 100.00 97.07 ( 320 J- 3 2 2 ) / ( 3 3 2 +33:4 ) CALC1`UL A TI ON R -G io o a ii 3) - .0729 < 3 2 8 ' >/< 332- * 3 3 ^> C A L C U L A T I O N K-G l o c a l i 3) - .5949 4r S ^ 1 C11037 File >B 3 133 333.6-334.6 amu 2UL UT-3057 SP2330 200-1/3/250 RUN ET F i l e >3133 3 2 1 .6 - 3 2 2 .6 amu.ZUL UT-3057 S P 2 3 3 S 2 0 0 - 1 / 3 / 2 5 0 RUN E T 4000 ""X-v'vV 2000- 0 I 1 1 1 1 I 1 1 -I--[--1--I--I--I--I--p- -T--|-- 1-- 1-- 1-- 10.0 10.5 11.0 11.5 12.0 i; 5 - i -- j-- i-- i-- i-- i i i-- i-- i-- I-- ]-- i . * ; <-- i < > - | 13.0 13.5 14.0 14.5 15.0 P ' o - r , ' - . . /" * i -- U. i i / , 0013! C11038 MS data file header from >B3133 Sam ple: 2UL UT-3057 O p e r a t o r : ROY MS 11/05/84 M i s e : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 RUN B T L # 7 7 B T L # 7 7 S y s . #: I M S mode 1 : 87- SW/HW r e v . : Cfi FILS # : 0 Method f i l e : SP2330 Tuning f i l e : fiPEI01 No.* o f e x t r a r e c o r d s : S o u r c e t e m p . : 248 final y z e r t ernp. : 0 T r a n s f e r lin e temp, 5 7 :3 4 Chromatgraphic tem peratunes : 0. 0. 0. 0. 0. "* C h r o m a t o g r a p h i c t i m e s - , m i n . : 0 . 0 0 . 0 0 . 0 0 . 0 0 . 0 Chromat ograph i c r a t e , deg/mi n : 0 .0 0 .0 0 .0 0 .0 0 .0 M/Z * 3 3 3 . 9 F i r s t peak i s b as e 1i ne drop c o r r e e t ed a r e a . Sec o nd p e ak i s t an g e n t skim m ed c o r r e c t e d a r e a . Peak # R. T. min. f ir st scan ma x scan 1a s t peak scan u i dt h raw area co rr. area co rr. 1 1 2 .4 1 5 253 259 271 2 1 2 .4 1 5 253 259 271 18 310151 18 310151 280291 253343 100.00 97.33 M/Z = 3 3 1 . 9 F i r s t p e ak i s b a s e 1 i ne drop c o rre c te d a re a . Second peak is t ange nt skimmed c o r r e c t e d a r e a . Peak # R. T. f i r s t mi n . scan max sc an 1a s t 'peak sc an w id th raw area co rr. area corr. % 1 1 2 .4 1 5 251 259 72 2 1 2 .4 1 5 251 259 272 21 277458 221556 100.00 21 2 7 7 4 5 8 ` 2 1 5 3 9 2 9 7 . 2 2 332/334 CALCULATION R -G lo b al< 0) = 8512 M/Z = 3 2 7 . 9 F i r s t p e ak i s b a s e l i n e drop c o rre c te d a re a . Second peak is tangent skimmed c o r r e c te d a r e a . *1 Peak # R .T. min. fi rst sc an nta x s can 1a s t peak scan width raw area co rr. area 1 12.435 254 260 273 2 12.435 254 260 273 19 3 4 5 5 6 2 8 6 4 4 5 19 345 5 16 2 8 0 0 7 0 M/Z = 3 2 1 . 9 F i r s t p e ak i s b a s e 1 i n e d r o p c o r r e c t e d a r e a ;. S e c o n d p e ak i s t a n g e n t s k im m e d c o r r e c t ed a r e a . Peak # R .T. f ir s t rni n . s c an max s can 1a s t scan peak w i d t It raw area 1 12.435 2 12.435 **w;; -, i 255 260 264 255 260 264 -- . #7 9 9 .....................\ l u ' 0 0 1 H 6 'J 1 f 'f-y i C , ^ i V E C E D E S . 30993 30993 c o rr. area 7215 4883 corr. y. 100.00 97.77 corr. V. 100.00 67.75 C11039 s M'Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak # R .T . mi n . fi rst scan max scan 1a s t peak s c a n u i'd t h r aui area 1 .-12.475 255 262 268 2 12.476 255 262 268 13 41741 13 41741 co rr. area 7967 7830 co rr. 5i 100.00 98.28 320/322 CALCULATION R - G 1o b a l < 1) = 1.1042 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak is tangen t skimmed c o rre c te d a re a . Peak # R .T. min. f i rst scan max scan 1a s t scan peak w id th raw area 1 0 000 2 0.000 269 269 0 268 0 268 -1 -1 0 0 corn. area 4058 4658 c o rr. % 100.00 100.00 ( 3 2 0 + 3 2 2 ) / < 3 3 2 + 3 3 4 ) C R L C U L R T I ON R-GlobalC 3) = .9315 C 3 2 3 ')/ (3 3 2 + 334) CALCULATION R - G 1o b a l < 3 ) = .5943 ooi ; 1J - C11040 r i l e >3134 3 3 3 .6 - 3 3 4 .6 *mu.2UL UT-3058 S P 2 3 3 0 2 O 0 - 1 / 3 / 2 5 0 RUN BT F i l e >3134 3 2 1 .6 - 3 2 2 .6 amu.SUL UT-305S S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN BT C11041 MS data fil header from >B3 134 Sample: 2UL UT-3058 O p e r a t o r : ROY MS 11/05/84 7:54 Mi s c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 6 RUN B T L # 7 9 B T L # 7 9 Bps. #: 1 MS m o d e l : 8 7 S U / H U r e v . i Cfl f l L S # : 0 Method f i l e : SP2330 Tuning f i 1 APEIOl No. o f e x t r a r e c o r d s : 2 Scure e t emp. : 250 A nalpser tem p.: 0 T ra n s f e r 1 i ne tem p. : 0 r Chromtographi c t em peratures : 0. 0. 0. 0. 0. Chromt ographi c t i mes, min. : 0 .0 0 .0 0 .0 0 .0 0 .0 Chromatographi c r a t e , deg/min: 0. 0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area. Second peak i s tangen t skimmed c o r r e c te d a r e a . Peak * min. f i rst s c an max s c an 1a s t peak sc an w id th raw area co rr. area corr. '4 1 12.386 247 257 269 2 12.386 247 257 269 22 311507 251975 100.06 22 311507 244627 97. 08 M/Z = 3 3 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d are a . Second peak i s t an ge nt skimmed c o r r e c t e d a r e a . Peak # R .T. min. firs t s c an max s c an 1as t peak sc an w id th raw area co rr, area co rr. * 1 1 2 . 3S6 251 257 269 2 1 2 .3 3 6 251 257 269 18 256725 212445 100.00 18 2 5 6 7 2 5 2 0 4 5 4 3 9 6 . 2 3 1- 1- cc (1 332/334 CALCULATION R - G 1o b a l ( 0> = .8431 M/Z = 3 2 7 . 9 F i r s t peak is b a s e lin e drop1 c o r r e c t e d a re a . Second peak i s tan g e n t skimmed c o r r e c t e d a re a . Peak # min. fi rst scan max s c an 1as t peak sc an w id th raw area 1 1 2 .4 0 6 251 258 267 2 1 2 .4 0 6 251 258 267 16 3 1 0 9 1 6 16 310916 M/Z = 3 2 1 . 9 F i r s t peak i s base lin e drop c o rre c te d ar ea . Second peak i s tang ent skimmed c o r r e c t ed a re a . Peak 4 R .T. min. f ir st sc an max scan 1 peak s c an w id t h raw area 1 1 2 .4 0 6 255 258 261 2 1 2 .4 0 6 255 258 261 6 6 n^ 24773 24773 ^o c o rr. area 258116 248116 co rr. '4 108.00 9 6 . 13 c o rr. ar ea 9185 7025 co rr. * 160.00 7 6 .4 8 C11042 M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. min. f i rst scan max sc an 1a s t peak sc an w id th raw area 1 ,1 2 .4 0 6 254 258 267 *2 1 2 . 4 0 6 2 3 4 2 5 8 2 6 7 13 4 2 6 8 3 13 4 2 6 8 3 7 ^ 3 1 3 y- c or r . area 8272 7979 co rr 100.0 96.4 3 2 0 / 3 2 2 C R L C U L f l T I OH R - G lo b a K 1) = . 9006 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o r r e c t e d a r e a . Second peak i s ta n g e n t skimmed c o r r e c t e d a r e a . Peak # R. T. min. Vi rst sc an max scan 1a s t peak sc an w id t h raw area 1 0.000 2 0.000 257 257 0 256 0 256 -1 -1 0 0 co rr. area 4558 4558 c o rr. 5. 100.00 100.00 ( 3 2 0 + 3 2 2 >/< 3 3 2 + 3 3 4 ) C A L C U L R T I ON R - G l o b a l C 3 ) =* .0376 < 3 2 8 0 / (3 3 2 + 334) CALCULATION R - G 1o b a l < 3 ) = .5556 a, C11043 F i l e >B 31 3 5 3 3 3 . - 3 3 4 . 6 a m u . 2 U L U T - 3 0 5 9 S P 2 3 3 0 3 0 0 - 1 / 3 / 2 5 0 RUN BT F i l e >B 3 1 35 3 2 1 , 6 --3 2 2 . 5 a m u . 2 UL U T --3 0 5 9 S P 2 3 3 0 2 O 0 - 1 / 3 / 2 5 0 RUN BT 4 0 0 0 ". / V - / ^ ^ 2060- " ! - r ' I-- i-- -- ' ' I '-- '-- 1-- 1-- |-- 1-- i-- '-- '-- I-- -- 1-- -- 1-- |-- i r -i p . i i-- i-- |-- i-- ,-- i-- ,-- |-- i-- 10.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 14.0 tn v w .. . ^VB rfr~ r C.DER. iw '.'1 4 1 ,-- p-- I-- i-- i-- i l | 14.5 15.0 C11044 MS data file header from : >B3135 Sam ple: 2UL UT-3059 O p e r a t o r : ROY MS 11/05/84 8:15 M i s c : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN B T L 4 8 1 B T L # 8 1 Sm s . #: 1 MS m o d e l i 8 7 S U / H U r e y . : Cfi R L S # : 0 Method f i l e : SR2330 Tuning f i l e RPEI01 No. o f e x t r a r e c o r d s : 2 Source tem p.: 248 R n a ly z e r temp. 0 T r a n s f e r lin e temp. : 0 rChromatographic tem peratures : 0. 0. 0. 0. 0. Chrom atographic tim e s, min. : 0 .0 0. 0 0 .0 0 .0 0 .0 Chromatographic r a t e , deg/min: 0 .0 0. 0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d area . Second peak is - ta n g e n t skimmed c o r r e c t e d a re a . Peak # R. T. min. fi rst s c an ma x scan 1a s t peak sc an w id th rau area c o rr. area corr. y. 1 12.372 2 12.372 252 252 259 259 268 268 16 238 5 76 16 238 5 76 198016 190888 100.00 96. 00 M/Z = 3 3 1 . 9 F i r s t peak i s base 1 i ne drop c o r r e c t e d a r e a . Second peak i s tangent skimmed c o r r e c t e d a r e a . Peak # R. T. min. firs t sc an max sc an 1a s t peak scan width rau area co rr. area co rr. y. 1 12.372 250 259 273 2 12.372 250 259 273 23 223423 23 223423 166153 161334 100.00 97.10 332/334 CALCULATION R-G lo b aK 0) = .8391 M/Z = 3 2 7 . 9 F i r s t p e ak i s b a s e 1 i n e drop c o rre c te d ar ea S e c o n d p e a k i s t ari g e n t s k i mmed c o r r e c t e d a r e a . Peak # R .T . min. f i rst scan ma x scan 1a st scan peak w id th raw area 1 12.393 2 12.393 255 255 260 260 271 271 1 258300 1 253300 M/2 = 3 2 1 . 9 F i r s t peak is bas e 1ine drop c o rre c te d a re a . Sec ond peak i s t an ge nt skimmed c o r r e c t e d ar e a . Peak 4 R .T. min. fi rst s c an ma x s c an 1 cl.S t pe ak sc an w id th raw area 1 12.393 12 ^393. --ECT TO^ 255 260 255 260 ---- f. 71 271 16 16 OD 46945 46945 9 co rr. area 212636 207076 co rr. ar ea 7441 353 co rr. % 100.00 97.39 co rr. 100.00 8 5 .3 8 C11045 S M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak # R .T. min. f irst scan max sc an 1a s t peak s c a n u i-dt h raw area 1 12.393 258 260 265 2 *' 1 2 . 3 9 3 5 8 2 6 0 2 6 5 7 23083 7 23883 ^ & 3 l3 S com . area 5359 5282 com . * 100.00 98.56 320/322 CALCULATION R - G l o b a l C 1> = , .7202 M/Z = . 2 5 7 . 0 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak is tangen t skimmed c o r r e c t e d a re a . Peak * R .T. min. firs t sc an max scan 1a s t peak scan width raw area 1 0.000 2 0.0O0 66 266 ,6 0 265 265 -1 -1 0 0 com . area 3787 3787 com . * 100.00 100.00 <320 + 3 2 2 )/< 332 +334) CALCULATION R -G lo b al< 3) = .0351 <3 2 S ' ) / ( 3 3 2 + 3 3 4 ) C A L C U L A T I O N R -G lo b al< 3) = .5837 i i : -4 4 \T -- C11046 rile >3136 333.6-334.6 amu.^UL UT-3073 S'P2 33Q 2OO-1/3/250 RUN BT File- >3136 3 2 1 .6 - 3 2 2 .6 amu.2UL UT-3073 S P 2 3 3 0 2 O 0 - 1 / 3 / 2 S 0 RUN BT 2000- F ile 0-j--r 10.0 >3136 n -- ]-- i-- i-- i-- :-- [-- i-- i-- i-- i-- |-- i-- n -- i-- j-- i-- i-- i-- r-|-- r- 10.5 11.0 11.5 12.0 12.5 319.6-320.6 amu.SUL UT-3073 T - ] --i--i--i--i--i--i--:--i--i--]--i--i--i--i--|--i--i--i--r-| 13.0 13.5 14.0 14.5 15.0 S P 2 3 3 0 2 D 0 - 1 / 3 / 2 5 0 RUN E T - --i i C11047 MS data file header from >B3136 Sampie 2UL UT-3073 O p e r a t o r : ROY MS 11/05/84 8:35 Mi s c S P 2 3 3 0 2 6 O - 1 / 3 / 2 5 0 RWN B T L # 8 3 B T L # 8 3 S y s. #: 1 MS m od e l : 8 7 SW/HW r e v . : Cfl R L S # : 0 Method f i l e : SP233Q Tuning f i l e : RPEI01 Ho. o f e x t r a r e c o r d s : 2 Source temp. : 248 f i n a l y z e r temp 0 Tran s f e r 1 i ne tem p. : 0 Chromt ograph i c t emperat u res : 0. 0. 0. 0. 0. / Chromt o g ra p h i c t i mes t m in. : 0 .0 0 .0 0 . 0 0 . 0 . 0 .0 Chrom atographi c r a t e , deg/min : 0 .0 0 .0 0*0 0 .0 0 .0 M/2 = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area. Second peak i s tangent skimmed c o r r e c te d a re a . P e ak # R. T. min. f irst scan max scan 1a s t peak scan u i dt h raw area com . area corr. * 1 1 2 .3 7 9 51 258 271 2 1 2 .3 7 9 51 258 271 20 281696 232916 100.00 20 281 6 96 2 2 8 6 9 6 9 8 . 19 M/Z = 3 3 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area . S e c o n d p e a k i s t a n g e n t s k i mmed c o r r e e t e d a r e a . Peak # R ,T. min. firs t sc an max scan 1a s t peak scan width raw area co rr. area corr. *4 1 12.379 248 58 270 2 12.379 243 258 270 22 246911 22 246911 193055 186488 100.00 9 6 .6 0 332/334 CfiLCULRTIOH R-G lo b aK 0) = . 8289 M/Z = 3 2 7 . 9 F i r s t peak is b a s e lin e drop c o rre c te d ar ea. Second peak is tangent sk im m e d .co rre cte d a re a . Peak # R. T. min. fi rst sc an max scan 1a st scan peak w id th raw area . * corr. area 1 12.399 2 12.399 247 247 259 70 259 . 270 23 297042 233677 23 297042 24943 M/Z = 3 2 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d ar ea . Second peak i s tangent skimmed c o rre c te d a re a . Peak # R .T. min. firs t s c an max scan 1a s t scan peak ui dt h raw area co rr. ar ea 1 12.399 2 12.399 i' 257 257 '' " 259 259 261 261. 4 4 001 ,/iS - > Vcj ~ C c ,jr C 0 P 3 Q 7 S C jiYE ORDER. 14562 14562 4314 3716 corr. * 100.00 9 6 .2 6 co rr. ym 100.00 8 6 . 14 C11048 S tl/Z = 319.9 First peak is baseline- drop corrected area. Second peak is tangent skimmed corrected area. F' e ak # R. T. min. firs t sc an max sc an 1a s t peak scan width raw area 1 12.399 252 259 268 2 1 2.399 252 259 268 16 44997 16 4 4 9 9 7 co rr. area 4901 4605 c o rr. * 100.00 9 3 .9 6 320^322 CALCULATION R -G lo b al( 1) = 1.1361 M/2 = 257.0 F i r s t peak is b a s e lin e drop c o rre c te d area. Second peak i s tan g en t skimmed c o r r e c te d a re a . Peak * R .T. m in. fi rst scan max scan 1a s t peak scan width raw area 1 0.000 2 0.000 269 269 0 263 -1 0 268 . . -1 0 0 co rr. area 3683 3688 corr. y. 100.00 100.00 (320 + 3 2 2 )/ (3 3 2 +334) CALCULATION R -G lo b al< 3) = .0216 ( 3 2 8 ') / (332 + 334) CALCULATION R-G 1o b a l( 3) = .5485 O r-t C11049 File > B 3 137 3 3 3 . 6 --3 3 4 * 6 am u 2UL 2.504/.43/.20 SP2330 20G-1/3/250 GT BT F i l e >3137 3 2 1 . 3 - 3 2 2 . 6 amu-.SUL 2 . 5 0 4 / . 4 8 / . 20 S P 2 3 3 8 2 0 0 - 1 / 3 / 2 5 0 GT BT \ n':`'a" SUBJECT TO PROTECTIVE ORDE \ C11050 MS data file header from : >B3137 Sam ple: 2UL 2 . 5 0 4 / . 4 8 / . 20 O p e r a t o r : ROY MS 11/05/34 M i s e S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 O GT BTL*41 BTL#41 S y s. #: 1 MS m o d e l : 3 7 SW/HW r e u . : Cft R L S # : 0 Method f i l e : SP2330 Tuning f i l e : RPEI01 Source tem p .: 243 fin alyzer tem p.: 0 Ho. o f e x t r a r e c o r d s : T r a n s f e r 1 i n e t e m p . e 8 :5 5 ?Chromatographic temperat ures : 0. 0. 0. 0. 0. Chrom atographi c t i flies, m in. : 0 .0 0 .0 0 .0 0 .0 0 .0 C hrom atograph!c r at e , deg/m i n : 0 .0 0 .0 0 .0 0 .0 0 .0 M/Z = 3 3 3 . 9 F i r s t peak is b a s e lin e drop c o rre c te d area . Second peak i s t arg en t skimmed c o r r e c te d a re a . P e ak '# R .T. min. f irst sc an max sc an 1a s t peak sc an w id th raw area co rr. area c o rr. v. 1 12.374 252 257 272 2 12.374 252 257 272 28 512301 464361 100.00 20 512301 457901 9 8 .6 7 M/Z = 3 3 1 . 9 Fi r s t peak is b a s e lin e drop c o rre c te d are a . S e c e n d p e a k i s t a n g e n t s k i mmed c o r r e e t e d a r e a . Peak # R .T. min. f i rst sc an max sc an 1a s t peak scan width raw area co rr. area corr. 7. 1 12.374 247 257 270 12;374 247 257 270 23 430776 375231 100.60 23 430776 367744 98. 00 3 3 2 / 3 3 4 C f i L C U L f l T I ON R - G 1o b a l < 0 ) = , 8036 M/Z = 3 2 7 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d area. S e c o n d pe ak i s t a n g e n t s k im m e d c o r r e c t e d a r e a . Peak # R .T . min. fi rst scan max scan 1a st peak sc an w id th raw area co rr. area c o rr. % 1 12.394 2 12.394 253 253 258 258 271 271 18 520261 471769 100.00 13 5 20 2 61 4 6 6 0 3 6 9 8 . 7 8 M/Z = 3 2 1 . 9 F i r s t peak i s b a s e lin e dr op c o r r e c t e d a r e a . Second peak i s t an ge nt skimmed c o r r e c t e d a r e a . Peak # P. T. min. fi rst sc an ma x =c a n 1a s t pe ak sc an wi dt h raw ar ea co rr, area co rr. X 1 12.394 246 258 271 25 2273243 2214793 1 0 0 .0 0 '2 1 2 .3 9 4 246 258 271 f'n * 25 a iD 2278243 2174668 9 3 . 19 C11051 h u t t r"-i s M/Z - 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R .T. min. fi rst scan max scan 1a s t peak sc an y i dt h rau area 1 -.12.394 249 258 272 2 12.394 249 258 272 23 1874580 23 1874580 >5313 7 co rr. area 1818986 1791136 co rr. y. 100.00 98.47 320/322 CALCULATION R - G 1o b a l < 1) = .8213 M/Z = 2 5 7 . 0 F i r s t peak i s b a s e lin e drop c o rre c te d area. Second peak i s tan g e n t skimmed c o rre c te d a re a . Peak # R .T. m in. firs t scan max s c an 1a s t scan peak ui dth rau area 1 12.394 2 12.394 250 250 258 258 273 273 23 1050625 23 1050625 c o rr. area 965341 955163 c o rr. 100.00 9 8 .9 5 <320 + 3 2 2 ) / < 3 3 2 + 3 3 0 C R L C U L A T I OH R -d o b a K 3) = 4.8061 < 3 2 3 0 / (3 3 2 + 334) CALCULATION R-G lobal< 3) = .5384 . SUBJECT. TO PROTECTIVE ORDER. C11052 File- >B313S 333.6-334.0 amu ..2JJL 25.04/,48/.20 SP2330 200-1/3/250 GT BT F i l e >B 3 138 3 2 1 . 6 - 3 2 2 . 6 am u .SU L 2 5 . 0 4 / . 4 8 / . 2 0 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT -BT SUBJECT TO PROTECTIVE ORDER. C11053 MS data file header from >B3138 Sam ple: 2UL 2 5 . 0 4 / . 4 8 / . 2 0 O p e r a t o r : ROY MS 1 1 / 0 5 / 8 4 9 : 15 M ise : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 GT BTL#43 BTL.H43 Sys. #: 1 MS m o d e l : 8 7 . SIJ/HW r e v . : Cfi f i L S # : 0 Method f i l e : SP2330 * Tuning f i l e : APEI01 No. o f e x t r a r e c o r d s : 2 Source tem p .: 250 A n a ly z e r tem p.: 0 T r a n s fe r lin e temp. : 0 ^Chromatographic tem peratures : Chrom atographic tim e s, min. : Chrom atographic r a t e , deg/min: 00 0.. 00. 00 0.. 00. 00 0.. 00. 00 0.. 00. 00 0.. 00. M/Z = 3 3 3 . 9 F i r s t peak i s b a s e lin e drop c o rre c te d are a . Second peak is .t a n g e n t skimmed c o r r e c te d a r e a . Peak * R. T. min. f i rst sc an max * 1a s t peak scan scan width raw area co rr. area co rr. % 1 12.402 245 260 268 2 12.402 245 260 268 23 594999 538235 100.00 23 594999 527287 9 7 .9 7 M/Z = 3 3 1 . 9 F i r s t peak is b a s e lin e drop c o rre c te d a re a . Second peak is tang en t skimmed c o r r e c te d a r e a . P e ak tt R .T . min. f i rst sc an max scan 1a s t peak sc an w id t h raw area co rr. area c o rr. * 1 12.402 253 260 275 O 12.402 250 260 275 25 496056 436156 100.00 25 496356 432081 9 9 .0 7 332/334 CALCULATION R -G lo b al< 0) = .8103 M/Z = 3 2 7 . 9 F i r s t peak i s b ase 1 i ne drop c o rre c te d a re a . Second peak i s t argent skimmed c o rre c te d a re a . . Peak # R .T. min. firs t scan max scan 1a s t peak s c a n wi dt h raw area co rr. area c o rr. % 1 1 2 .4 2 2 252 261 273 2 1 2 .4 2 2 252 261 273 21 819857 767294 108.00 21 8 19 8 5 7 7 5 9 3 7 7 9 8 .9 7 M/Z = 3 2 1 . 9 F i r s t peak i s base 1ine drop c o rre c te d a re a . Second peak i s t angent skimmed c o r r e c te d a r e a . Peak R .T . min. f i rst sc an max s c an 1as t peak sc an w id t h raw area co rr. area co rr. 1 1 2 .4 2 2 252 261 270 2 1 2 .4 2 2 252 261 270 IS 25792552 25748148 18 2 5 7 9 2 5 5 2 2 5 4 0 7 9 7 2 130.00 98.68 SUBJECT TO PROTECT >7 l ,-r i ."'Y -'.u i r^r: ---- C11054 S M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R .T. min. fi rst scan max' sc an 1a s t peak scan width raw area c o rr. area 1 , 12.442 249 262 272 2' 12.442 249 262 272 23 21171796 21112984 23 21171796 20842836 7 f3 )3 ^ corr. 100.00 9 8 .7 2 320/322 CALCULATION R - G 1o b a l ( 1) = . 8200 M/Z = 2 5 7 . 0 F i r s t peak is b a s e lin e drop c o rre cte d area. Second peak i s tan g e n t skimmed c o rre c te d a re a . P eak # R .T. min. fi rst scan max scan 1a st peak s c a n wi d th raw area 1 12.442 2 12.442 250 250 262 262 274 274 24 11339399 24 11339390 c o rr. area 11262638 11137286 corr. y. 100.00 9 8 .8 9 C3 2 0 + 3 2 2 ) / C3 3 2 + 3 3 4 ) C A L C U L A T I O N R-G1obal< 3) = 4 8 .0 9 2 7 < 328')/< 332 + 334) CALCULATION R-G lobal< 3) = .5496 il SUBJECT TO PROTECTIVE ORDER. r'\ r . M -f C11055 9 3 3 3 . 6 - 3 3 4 * 6 amo. DODECAHE S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN BT -- i-- j t i 7 ~ i-- i-- i-- i-- |-- i-- i-- i-- i-- |-- r i- i i |-- r ~ r .0 10.5 11.0 1 1 .S 12.0 39 3 3 1 . 6 - 3 3 2 .& a m u . CODEGONE 12.5 . t -- t t j t i r i - 1 - i t i - r " [ t r - i-- i-- j 13.0 13.5 14.0 14.5 15.0 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN BT 22732,64 date ,0 6 0 ^ C>-tC. ' 139 3 2 1 .6 - 3 2 2 .6 amuDODECRNE SP 233 2 0 0 - 1 / 3 / 2 5 0 RUN BT '6 J L +a ^ ^ ^ S ' aJ 1 J C?" *?:.... \SUBJECT TO PECTICr.V/Er-- c r d e : C11056 5 -y / / K - / date ' J7 -- S S U2 :0 / a iv a a a o e itM iQ N n o n v o v im SOTTO 'M a a t t o 3 A I 1 0 1 L Q I J 6 j i 3 ~ r c , . b r v V.--t --r' - f m * SS* y b jj 'p lr t} ip tr^ o x L - o = ^ Q ^ -Jr $-* < f l f f f Tf r ,y C L ^ 7 7 ^ j? < ? y ^ y t ? - C ? if - ^ * - 7 7 * * ^ ' F " S < p f s p f f i I f l f i r L q .0 fr - f t * ? *~y~ Loeyo -.. >4V( r ~J- -0*0/ < f f f i f l^L P O 'jr f gr7 ip - ^ ip o 's - r - / r * o / <% f * m ' r f~ L '< & r t * i 1 " ^ ^ p rwA7 jy f - Jit f- r j. p 'S ' i f / 1 r> *. ' * / v T r f r l* ' ^ A > 7 a?/ cjk /pffypy g f r L - f r ic Y T /w 2 r T * : " p fP ^ *p r / y ^ * * - P T - 0 -^ 7 ja f f a t . /~ 'M ? ^ A >! T&) dlit. oA/' ^ T r ^ p y '.', ^ / w r y C Ld ^ -C -T p c 3 7 * > ^ ? <? / * * ^ i r ^ x i i y * # r Y 6 : ^ f r w jp (T f v 4 *vA ) - '9vs7? r-r> ' 7~i^rfp ~ r ' . S r t ' / t n f Q ^ &*&<?/ S?J?^P5'Zy 'v/ty o / .- m - X -oj* J p i ^ZiL-TD n 2 _ 0 ' S - -a^ 9 f y _ ^ - - y / x - O / r ~ -frWo / _ ^ ffir lp Q * ^ L 'O O ^ -- <<SZ<$53JJ--J * f p y / i &>< 9 0 0 0 V - << Zj?3ofijipj?iSgZ^0 Wh t t^jgfooiOo Oo o /J^ - * - ~ T ^ Jl, ~ i- -3 Lj. <&h ' 7v/// ^ 7^ * 7 4 ^ ^ ^ 'O " ^ p ^ ' ' <3$ 7s /po x siva T92G22 N vmkjl ________tsyWivivN S io as ataaWw>Vds3d //< 7 0 / ` U t , ^v i ' ANVdWOO OINVSNOW on s o r losrans MONSANTO COMPANY N? 2273265 SU BJECT JO B NO. i V" ^ c > A j 2 " S a l. l o o / / :; ; / lu j 1 7 AilJjkfti*&' P R E P A R E D B Y (SIG f4f T U R E ) X ^ l m .____________ DATE 17 o c 7 S '/ M / d J L J J&tyU0C-/'1tr sJ. !L - ? y 'tjig'h/tc^dL h JL StOcfl - 1 -f i i f /,*o 2 & $ o c n .o 3 -- o , w y ,,/ ^ ^ - /o. o t / y ? ' C / s o ^ d i /(* X . o o b - / . o o ? ' ' c : / v ? ' c </ 3 o ' l 'c e V / J - < .^co - O .lo d i 'V V r / 0 / 0 % < M ' - b / r o zrd l d J L J o. c o - JU iS a J % / c jJ L --4 tdU ~ 'L d7S>b C*-~. - O .oioo^ c/.V t/jc,- l'r j.jk ie J p ji-h - / / k t* - ~ J ~ tJ L - & lolliCl 1 3 H 5 C . O / 3 0 "C- / Vs" `V / j o 31ci2 0 . 3l O ..3. S 0Y } . Co 2.5oV ^ 7 S.S. 'i s /?<?^ o.?yA>i4 "c / i o >rtJ? ? ) i i " iO J '* c o. y ^ J ! r ..A. ~ / c u "<l o . f L j~ J L - -3JE C T TO PROTECTIVE O R D "^ C11058 R ( * Q AMO UMDCRITOOD T DATE '